MICROCHEM.fr
Non Profit Organization to boost your fine chemical process from lab to industrial unit
M. ALAS C.E.O.
Asking for inquiries ? : alas@microchem.fr
| MICROCHEM.fr Non Profit Organization to boost your fine chemical process from lab to industrial unit
M. ALAS C.E.O. Asking for inquiries ? : alas@microchem.fr | |
| Alas patents recap: |
| HIGH-TEMPERATURE CHEMISTRY |
 Laboratory and pilot-scale study of the production of various ketones through the continuous decarboxylation of acids or diacids at 250-500°C using ad hoc catalysts to obtain the corresponding ketones. Screening of catalysts and operating conditions (Brevet FR2800066 ) (Brevet US5856581 ) (Brevet US 5600013 ) with pilot testing. Assistance with the industrial implementation for the production of the first thousands of tons. |  Laboratory study, piloting, and monitoring of the industrial production of the first tons of 2,3 pentane dione meeting perfumery quality standards via continuous decarboxylation of lactic acid on ad hoc catalysts at 220°-280°C.(2,3pentane dione info) |
 Laboratory and pilot study of the production of 2-cyanophenol through continuous reaction at 400°C in the vapor phase of methyl salicylate with ammonia, followed by selective isolation to achieve the client’s required quality. (Brevet US 2006149093) .Building block for agrochemicals like azoxystrobin (herbicide from Zeneca now Syngenta) and many pharmaceuticals (more info) |  Development in the lab and pilot scale of a new method to activate a copper-based dehydrogenation catalyst. Extrapolation to the client's industrial unit (Spain), start-up, personnel training, and performance monitoring (application: continuous vapor-phase dehydrogenation of cyclohexanol into cyclohexanone in units producing caprolactam, an intermediate for nylon 6 ).(proc 93,206) |
| PRODUCTION OF VARIOUS ESTERS |
 Ethyl orthoformate/Methyl orthoformate : Development in the lab and at pilot scale of a 2 steps process starting from cyanhydric acid, ethanol/Methanol and hydrochloricic gaz (Pinner synthesis followed by ethanolyse of the imino ester ) , supplying engineering and technical data to build the new unit ,Technical assistance for unit start up and production follow up for the first 500 tons (usage : Intermediate for various products like chloroquine and many others like Azoxystrobin . update1 chloroquine , orthoester chemistry info , ,,,,, | Ethyl propionate:
Development of a continuous process in the lab and extrapolation to an
existing installation. Monitoring of the initial industrial productions. Ethyl oxalate: Development of a continuos process that halves the energy consumption of the production unit. Ethyl formate: Productivity improvement of a continuous production unit from effluents containing formic acid. Methyl oxalate: Development of a continuous process and implementation in an existing unit.(proc 182) |  Butyl acetate / Isobutyl acetate: Optimization of the esterification reactor's operation using ion-exchange resin catalysts to increase productivity. Modification of the installation to reduce corrosion. Monitoring performance during the production of the first thousands of tons. |
 2-Acétoxy-1-méthoxypropane:: also known as methoxypropanol acetate (alias DOWANOL PMA) Definition in the lab of the operating conditions and resin catalyst for a continuous process . Extrapolation to an existing unit. Start-up of the installation and assistance for the production of the first thousands of tons.('main use : solvent ,the combination of an ester and an ether functional group in the same molecule provides unique solvency characteristics ). (commercial notice) |  Ethyl sodium oxalacetate Development of a simplified process in the lab to obtain this product from ethyl oxalate, ethyl acetate, and metallic sodium. Industrial implementation in an existing unit. Monitoring the production of the first hundreds of tons. |  Development of an industrializable process without investment in an existing unit of a methyl vanillate production in 2 chemical steps . Industrial implementation and assistance with the production of the first tons. (see main use) |
 Development in the lab of a continuous process for 2-Hydroxy-4-(Methylthio) Butanoic Acid Isopropyl Ester (HMBI, an animal feed additive (HMBI info ) ) adaptable with minimal investment in an existing unit.(customer ADISSEO now ChemChina) Sizing of the main equipment. Monitoring the production of the first tons in an existing multipurpose workshop. |  |  Isoamyl acetate: Continuous process Optimization of the resin catalyst to increase productivity. Modification of the process to make it operable in another unit.(FOOD ADDITIVES PERMITTED FOR DIRECT ADDITION TO FOOD FOR HUMAN CONSUMPTION) |
 proc 32Methyl phenyl glycidate d'ethyle Development of a manufacturing process starting from acetophenon/chloropropionate/EtONa, extrapolation for an existing unit, monitoring of the start-up () (main use = strawberry aroma) mpge info |  Development in the lab and extrapolation to existing units for the production of diethyl methyl malonate in two chemical phases from metallic sodium, ethyl oxalate, and ethyl propionate. Assistance with the production of the first tens tons. |
| SALICYLIC ACID DERIVATIVES |
 Laboratory study and scaling up in an existing unit for the production in continuous of salicylic acid esters with various alcohols ranging from methanol to isoamyl alcohol. |  Laboratory study and scaling up in an existing unit of a new process for manufacturing salicylamide with high volumetric productivity. Assistance with the start-up for the first hundreds of tons. |
 Laboratory and pilot study of a continuous process for the production of hydroxybenzonitrile by vapor-phase dehydration of ammonium salicylate. Lab study of direct synthesis of cyanophenol in 2 chemical steps starting from phenol ,formaldehyde, ammonium derivatives and catalysts |  Laboratory and pilot study of a process for producing salicylic aldehyde by condensation of formaldehyde on phenol catalyzed by zinc salts followed by catalytic oxydation .(salicylaldehyde update) |
| TRIFLUOROACETIC ACID DERIVATIVE |
Methyl/ethyl/isopropyl trifluoroacetate: laboratory development of a simplified operating procedure. Implementation in an existing unit. Assistance with the production of the first tens of tons. | trifluoroacetamideTrifluoroacetamide: laboratory study. Pilot production for sampling. |
 |  proc 174Trifluoroacetic anhydride: laboratory study of a simplified process starting from trifluoroacetic acid. Scaling up to an existing multipurpose unit. Assistance with the production of the first tons. |
 Trifluoro acetyl acetone: development of a process in the laboratory. Pilot implementation for customer sampling. |  Allyl trifluoroacetoacetate: development of a process in the laboratory, scaling up in an existing multipurpose workshop, and assistance with the production of the first tons. |
| N-trifluoro acetyl-L-Lysine (CAS :10009-20-8) : development of an
operating procedure in the laboratory from methyl trifluoroacetate and
L-lysine. |
| GREEN CHEMISTRY |
 Improvement of the industrial extraction process of D-lactic acid obtained by fermentation (increased productivity and reduced energy consumption), monitoring the performance over the first thousands of tons. |  Development in the lab and then at pilot scale of a process for the extraction/purification of natural vanillin obtained by fermentation of ferulic acid (e.g., from rice). Scale-up in existing units and support for the production of the first tons of product (Rhovanil Natural).(flavor usage) |
Development in the lab and at pilot scale of a process for the production of esters from the ammonium salt of the corresponding acid, the latter being obtained by fermentation. Application to D- lactic acid esters, with a process that generates no effluents, as all reactants and by-products are fully recycled and racemization kept at low level (Brevet EP0517571). |  Lab and pilot scale development of the extraction/purification of pipecolic acid obtained by biotransformation of L-lysine using a microorganism. |
 Study of an industrial unit for the production of 10 natural amino acids by separating the components of a hydrolysate of protein materials from animal origin (chicken feathers or hog bristle ). |  Development in the lab and scale-up in an existing unit for the production of citraconic anhydride by thermal dehydration of itaconic acid (also known as methylene succinic acid) obtained by fermentation . |
 Study of a process for synthesizing itaconic anhydride by continuous thermal anhydration of a fermentation broth (Brevet EP 0749952 ). |  Lab and pilot scale development of a process for isolating brassylic acid (a raw material for the perfume industry) obtained by fermentation, and scale-up in existing facilities. |
  Lab development and scale-up in an existing multipurpose unit for the chemical modification of guar gum to impart the desired properties for the target markets (mainly cosmetics JAGUAR C162 ,JAGUAR EXCEL ... ). Support for the production of the first hundreds of tons of various required qualities . (modified guar info ) .Modifiying guar flour to meet viscosity constraint (meyprogat 150 proc 95) |   Development of a process for bacterial decontamination of carob flour (also known as locust bean gum), a natural hydrocolloid, to meet food-grade specifications. Support for the production of the first tens of tonsin an existing unit .(proc 193) (guar vs carob) |
| Development of a continuous esterification process of
D-lactic acid from fermentation with alcohols ranging from methanol to
isobutanol and implementation in an existing industrial unit (brevet EP0287426 ). Support for the production of the first hundreds of tons. | Development of a process for producing ultra-pure D-lactic acid (monomer for biocompatible polymer) through ester hydrolysis. Implementation in an existing multipurpose facility for the first tons of production. |
 Development of a three-phase process for producing sodium erythorbate (sodium isoascorbate) from a raw fermentation broth . Scale-up to an existing unit. |  Improvement of the quality of natural amyl alcohol obtained by distillation of fusel oil (a by-product of natural ethanol distillation) (fusel oil info) . Optimization of distillation conditions to improve quality and maximize recovery of propanol, isobutanol, and butanol, all of which carry the natural label. |
Lab development and industrial-scale implementation in an existing multipurpose unit for the production of itaconic anhydride (an intermediate for varnishes in the electronics industry and UV resitant paints ) from itaconic acid obtained by fermentation and acetic anhydride. Support for the production of the first tens of tons. Development of an effluent-free process via direct dehydration of itaconic acid on modified natural clays .(Brevet FR2623500) |  |
 proc 160Lab development and implementation in a multipurpose workshop for the production of citronellyl lactate from fermentation-derived D-or L+ lactic acid for use in perfumery ( ROSILIAL +) .(more info1) |  Development of a rustic process for a multipurpose unit to make hydroxy propyl beta cyclodextrine with adjustable substitution ratio from betacyclodextrine so as to adjust its solubility power (info1) |
recovery of solvent mixtures from electronic industry in existing unit (continuous or batchwise)(pro 191) or direct utilization for other purposes |
| CATALYSIS PRODUCTS |
| Development in the lab and pilot scale of the production of rare earth carboxylates (mainly Cerium,Neodymium, Lanthanum), leading to the finished product either in liquid form (Brevet WO 9954335 ) or in powder form (Brevet WO 9839283) . Assistance in the production of the first several tons (used in Ziegler-Natta polymerization of various monomers such as butadiene). | Lab development of a catalyst based on cerium oxide nanoparticles for reducing pollution from diesel engines. Development of an industrializable process in the lab, pilot testing, and extrapolation in an existing multipurpose workshop to ensure the production of the first several tons (product marketed under the name EOLYS DPX 42 (Particle filter info ) |
Development of a simple and productive process for manufacturing Cerium stearate, transposable to an existing workshop, with assistance for the production of the first several tons.(catalysis for agricultural plastic decomposition) | Development of a chrome oxide (Cr2O3)-based catalyst and implementation in an existing workshop.(proc 123) :usage : multi purpose oxydation catalyst . |
Development in the lab and pilot scale of a new method to activate a copper-based dehydrogenation catalyst. Extrapolation to the client's industrial unit (Spain), start-up, personnel training, and performance monitoring (application: continuous vapor-phase dehydrogenation of cyclohexanol into cyclohexanone in units producing caprolactam, an intermediate for nylon 6 ).(proc 93) |
| CONTINUOUS HYDROGENATION UNDER PRESSURE |
 Improvement of existing processes for synthesizing various aliphatic amines through continuous aminative hydrogenation under pressure of various aldehydes and ketones in the presence of ammonia or various amines to produce the corresponding amine (furfuryl amine,, methyl butyl amine,cyclopentyl amine... ). |  Lab and pilot-scale development of the production of TDA1 , a cost-effective and environmentally friendly crown ether, from methyl diglycol, ammonia gas, and hydrogen in continuous flow over a fixed bed catalyst . Scale up in an existing unit ,assistance for industrial startup to produce the first several tons .(Brevet US 6403834) more info on TDA-1 HERE |
| Lab development followed by pilot-scale implementation of a continuous process for the production of Gilotherm D12
(a heat transfer fluid) through continuous hydrogenation of propylene
tetramer. Commissioning in an existing facility and assistance for
production. | Development of a continuous hydrogenation process using a nickel-supported catalyst for ortho-cresol to produce ortho-methyl cyclohexanol. Extrapolation to an existing unit. |
 development at pilot level of the continous hydrogenation of styrene oxide into stryralil alcohol for the perfume industry |
| ADDITIVES FOR PVC PROCESSING INDUSTRY |
 Development in the laboratory of a manufacturing process for various betadiketones used as stabilizers in PVC processing, starting from metallic sodium with various esters and ketones .(Brevet FR 2842519) (Brevet FR 2843400 ) Monitoring and assistance for industrial production of the first thousands of tons (RODIASTAB range: RH50, RH83,RH2000). |  Adaptation in the lab of a UK-origin manufacturing process (AKZO-F6) in 4 chemical steps starting from aniline to produce a PVC stabilizer. Extrapolation to an existing unit, assistance for the production of the first tons.(proc 196) |
 Lab development followed by pilot and then industrial implementation of a simple process (one step synthesis sarting from acetyl acetone) for manufacturing metal acetylacetonate (metal=calcium or zinc) for the PVC industry. Assistance for the production of the first hundreds of tons .(brevet FR2798381 brevet FR2775971 ). |  Development at lab level of a manufacturing process to make 5 methyl 1 phenyl hexane 1,3 dione (CAS number13893-97-5) , a liquid PVC stabilizer .Scaling up for an existing industrial unit and Follow up for the first 10 tons (usage example) |
 Dialkyl thiomalate PVC costabilizer : Development in the laboratory of the manufacturing process of various esters of thiomalic acid obtained by the addition of hydrogen sulfide to different esters of maleic acid. .(example of use as PVC stabilzer) ,( other use) |
MANUFACTURING OF VARIOUS CHEMICAL INTERMEDIATES |
 Lab development followed by industrialization in a multipurpose workshop of the production of carboethoxy cyclohexanone in 2 chemical phases from cyclohexanone and ethyl oxalate. Assistance for the production of the first several tons (pharmaceutical intermediate). | Lab development of the production of ethyl hydroxybutenoate, a synthesis intermediate for an herbicide under development for a Japanese client, obtained in 2 chemical phases starting from acetone, ethyl chloroacetate, and sodium ethoxide. Improvement of the conditions (Brevet WO9858898 ). Extrapolation to an existing multipurpose unit. Monitoring and assistance for the first tens tons produced. |
 |  Laboratory development of a manufacturing process to get a solution or suspension of various alkoxides from liquid sodium and the corresponding alcohol (Methanol / Ethanol/ t-Amyl Alcohol,t butyl Alcohol ), adapted for existing units, technical assistance for the start-up. Use: chemical intermediate for onsite use |
 dimethylsuccinylsuccinate DMSS : Improvment of a batch process( self condensation of 2 moles of dimethyl succinate) made in a multi purpose unit to boost productivity and meet quality standard for the customer (dye industry) |  pro208Batch process to make 2 methyl cyclopentanone in 3 steps starting from dimethyl adipate .for a dedicated unit |
| Pharmaceuticals |
 Development of a new manufacturing process for calcium leucovorin (calcium folinate) , an antidote for various anticancer drugs and methanol intoxication, starting from folic acid .Implementation of the process in an existing multipurpose unit (more info). |  Improvement of existing industrial process of extraction and purification for daunorubicin obtained by fermentation , improving of the recovery yield from broth to final product |
 Development of the manufacturing process for Detorubicine (CAS 66211-92-55) anti mitotic drug) in 5 phases starting from daunorubicin. Operation at pilot level to supply the first kilogram for clinical trials .(more info on detorubicin) |  |
| Agrochemicals |
 Technical assitance for the start up of an industrial unit manufacturing Oxadiazon (an herbicide still marketed by BAYER company under the name RONSTAR) in 7 phases integrated on the same industrial site (oxadiazon info). Definition of actions and monitoring their implementation with the local engineering team to achieve the objectives in terms of performance quality and productivity. Writing of the complete operating manual and engineering assistance for a duplicated unit in Japan with a japanese partner (formerely SHOWA DENKO K. K.). ( chemical route details ) |  Collecting technical information on fabrication of BIFENOX ( chemical route (Bifenox info1), , info2 ,info3) an herbicide for wheat ,operating on a small scale in Mount Pleasant (Tn USA) .Gathering technical and historical informations about the process and writing the process book so as to scale it up in another plant elsewhere update1 Product marketed by ADAMA Ltd under name FOX (update2) |
Development of a manufacturing process in 4 phases from dichloro aniline for IPRODIONE (alias RP26019) anti fungal chemical currently marketed under the name ROVRAL by the BASF company (info IPRODIONE). Defining process at lab level, piloting the process and industrial assistance for the production of the first tons of active ingredient in existing units located in various locations in France.(chemical route)  |  Development at laboratory level of a DIMEFURON manufacturing process starting from 3,5-dichloronitrobenzene in 5 phases, adapted so as to be operated in existing equipments . Technical assistance for the production of the first tens of tons (dimefuron usage) , (update_1) ( chemical route ), |
 |  Evaluate at lab level various chemical routes to make ACIFLUORFEN from readily available materials (toluenechlorine/HF/nitric acid...) |
| MONOMERS AND POLYMERS |
 Transposition to an existing unit of a US manufacturing process for a cationic polymer, MIRAPOL A15, obtained in 2 chemical phases from dimethyl amino propyl amine and dichloro ethyl ether (MIRAPOL A15, also known as MIRAPOL A15 alias POLYQUATERNIUM-2) . Modification of the process to increase productivity and achieve a quality compatible with the requirements of the cosmetic market. Monitoring performance and assistance for the production of the first hundreds of tons. |  Transposition of a process used in a US plant for manufacturing SIPOMER WAM in 2 consecutive chemical phases in an existing workshop(Diethylene triamine/urea/allylglycidyl ethl ether). This product, copolymerized with various acrylic monomers, improves the adhesion of the resulting products (latex paint applications). Gathering information, defining necessary modifications, training personnel, and assisting in the production of the first hundreds of tons to meet quality and productivity goals. |
 |  Lab and industrial pilot study of a process for valorizing residual acrylic acid into purified butyl acrylate. Monitoring pilot production of 50 tons in an existing unit. |
. |  Lab process for manufacturing Dicyclopentadiene methacrylate from dicyclopentadiene and methacrylic acid in a multipurpose unit (proc 201) |
| PROCESS LICENCE SALE |
 Vapor phase hydrogenation process of furfural to furfuryl alcohol and methyl furan over a copper catalyst: Writing of the process book, sizing of main equipment based on client specifications, discussions with partners, and on-site startup assistance (Wuji Furan Chemical, Hebei, People's Republic of China). | Vapor phase dehydrogenation process of cyclohexanol to cyclohexanone for caprolactam units (Nylon 6 monomer): lab and micropilot improvement of an existing catalyst (Cu640) to meet client specifications, writing the process book tailored to client unit specifics, and on-site startup assistance (UNIVEX Mexico(proc150) , Monoméros Salamanca plant Colombia, Hankook Ulsan Plant South Korea, Proquimed (proc 121) , now UBE Castelon de la Plana Plant in Spain). |
| DOWNSTREAM ETHANOL CHEMISTRY PROCESSES |
Production of acetic anhydride by thermal dehydration of acetic acid Production of acetic anhydride by oxidation of acetaldehyde butyraldehyde by liquid-phase hydrogenation of crotonaldehyde Production of butyl chloride from butanol and hydrochloric acid Production of ethyl ether by dehydration of ethanol. | Production of acetaldehyde by continuous dehydrogenation of ethanol Production of acetaldehyde by oxidation of ethanol Production of crotonaldehyde from acetaldehyde Production of butanol by hydrogenation of crotonaldehyde butyraldehyde by vapor phase hydrogenation of crotonaldehyde Production of ethyl hexanol from butyraldehyde |
| Unclassified manufacturing process |
 Cosmetic market ,proc154Batch process to make parsol 1789 ( alias 1-(4 ter butyl-phenyl)-3(4methoxy-phenyl)-propane -1,3 dione alias AVOBENZONE, CAS 70356-09-1 see other names ,) in a multi pupose unit starting from aceto anisol and para tertio butyl methyl benzoate , main application : cosmetic market ,sunscreen product for protection against UV radiation (example of application) |  process 64 |
 food additive proc211continous estérification process of isobutyrique acid to phenoxy ethyl isobutyrate (main use) |  cosmetic market pro202Batch process to make Geranic acid by chemical oxidation of geranial |
 proc 145, 149Vanillic acid by chemical or catalytic oxydation of vanilline for a multipurpose unit (main use food additive) (see other uses) | Continuous/Batch process to produce citral (mixture 50/50 of geranial and neral) from isoprene in 4 chemical steps ( process details ) |
 Batch process to produce citronellal from citral (process info) |
Production of isopropyl acetate by acetylation of propylene Production of acetone by dehydrogenation of isopropanol Production of diacetone alcohol by ketonization of acetone | Production of mesityl oxide by crotonization of diacetone alcohol Production of mesityl oxide by ketocrotonization of acetone Production of methyl isobutyl ketone by hydrogenation of mesityl oxide |
| Production of metal catalysts (Copper, Nickel, Chrome) on various supports | isopropyl ether by hydration of propylene isopropanol by hydration of propylene |