CN102381973A - Production process of ultra-high purity (electronic grade) lactate product - Google Patents
Production process of ultra-high purity (electronic grade) lactate product Download PDFInfo
- Publication number
- CN102381973A CN102381973A CN2011102777779A CN201110277777A CN102381973A CN 102381973 A CN102381973 A CN 102381973A CN 2011102777779 A CN2011102777779 A CN 2011102777779A CN 201110277777 A CN201110277777 A CN 201110277777A CN 102381973 A CN102381973 A CN 102381973A
- Authority
- CN
- China
- Prior art keywords
- lactate
- flasher
- cat head
- tower
- column
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000005342 ion exchange Methods 0.000 claims abstract description 16
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 15
- 229910052799 carbon Inorganic materials 0.000 claims abstract 2
- 241000282326 Felis catus Species 0.000 claims description 39
- 238000000605 extraction Methods 0.000 claims description 33
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 32
- 229920005989 resin Polymers 0.000 claims description 29
- 239000011347 resin Substances 0.000 claims description 29
- 239000000126 substance Substances 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 150000003903 lactic acid esters Chemical class 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 26
- 229920001429 chelating resin Polymers 0.000 claims description 23
- 238000011049 filling Methods 0.000 claims description 20
- 238000012856 packing Methods 0.000 claims description 20
- 238000003860 storage Methods 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 235000014655 lactic acid Nutrition 0.000 claims description 16
- 239000004310 lactic acid Substances 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000012535 impurity Substances 0.000 claims description 11
- -1 metals ion Chemical class 0.000 claims description 11
- 239000007791 liquid phase Substances 0.000 claims description 10
- 239000003463 adsorbent Substances 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 9
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 8
- 244000060011 Cocos nucifera Species 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 235000013305 food Nutrition 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000013461 design Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 239000000049 pigment Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000009849 deactivation Effects 0.000 claims 1
- 230000006837 decompression Effects 0.000 claims 1
- 239000012498 ultrapure water Substances 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 37
- 238000004042 decolorization Methods 0.000 abstract 1
- 238000006356 dehydrogenation reaction Methods 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 238000011268 retreatment Methods 0.000 abstract 1
- 239000011265 semifinished product Substances 0.000 abstract 1
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 36
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 30
- 229940116333 ethyl lactate Drugs 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- MRABAEUHTLLEML-UHFFFAOYSA-N Butyl lactate Chemical compound CCCCOC(=O)C(C)O MRABAEUHTLLEML-UHFFFAOYSA-N 0.000 description 15
- LPEKGGXMPWTOCB-UHFFFAOYSA-N 8beta-(2,3-epoxy-2-methylbutyryloxy)-14-acetoxytithifolin Natural products COC(=O)C(C)O LPEKGGXMPWTOCB-UHFFFAOYSA-N 0.000 description 14
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 14
- 125000002091 cationic group Chemical group 0.000 description 14
- ODQWQRRAPPTVAG-GZTJUZNOSA-N doxepin Chemical compound C1OC2=CC=CC=C2C(=C/CCN(C)C)/C2=CC=CC=C21 ODQWQRRAPPTVAG-GZTJUZNOSA-N 0.000 description 14
- 229940057867 methyl lactate Drugs 0.000 description 14
- 229940017144 n-butyl lactate Drugs 0.000 description 14
- 229910001220 stainless steel Inorganic materials 0.000 description 14
- 239000010935 stainless steel Substances 0.000 description 14
- 239000007788 liquid Substances 0.000 description 7
- 239000010903 husk Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000004821 distillation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- LCTONWCANYUPML-UHFFFAOYSA-M Pyruvate Chemical compound CC(=O)C([O-])=O LCTONWCANYUPML-UHFFFAOYSA-M 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229920006397 acrylic thermoplastic Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000000779 depleting effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a production process of an electronic grade lactate product. The production process is composed of a flash evaporation system, a dehydrogenation rectification system and a semifinished product rectification system, an active carbon decolorization system and an ion exchange system. The lactate recycling rate in the whole process is more than 98%, the lactate purity reaches as high as 99.9999%, the metal ion content is less than 3 ppb, and the lactate is colorless. The production process can completely satisfy the high requirement of the electronic industry. The light component in the flow is returned to a flash evaporator for retreatment, the heavy component in a second tower is intensively treated, therefore, the finished product yield is greatly improved, the residue discharge amount is reduced, the economical efficiency of the process is improved, and the treatment cost of the process is lowered.
Description
Technical field
The present invention relates to the production technique of a kind of ultra-high purity (electronic-grade) lactic acid ester product.
Background technology
Lactic acid ester mainly refers to methyl lactate, ethyl lactate and n-Butyl lactate, the lactic acid that to be carbohydrates such as lactose, starch produce through lactobacillus-fermented respectively with the product of methyl alcohol, ethanol and esterified by butyl alcohol.Lactic acid ester is one type of biodegradable and nontoxic solvent; Has the ability that substitutes some conventional solvent; Because it has many good physical and chemical performances, such as: (1) has fabulous dissolving power to resin (nitrocotton, acrylics, polyurethane(s), polyester, Synolac, epoxy resin etc.); (2) in water higher relatively solubleness and in most of organic solvents good solubility; (3) low relatively volatility makes it can be effectively applied to surface treatment; (4) high relatively boiling point can be effectively applied in the hot environment it.Lactic acid ester not only can use but also can be used as the prescription of cleaning solvent separately, was used for the cleaning of multiple precision optical machinery and carried out the cleaning before the face coat.It is little that lactic acid ester has in the use loss as clean-out system, and good economy performance has no adverse effects to being cleaned thing, and is nontoxic, and advantages such as readily biodegradable are a kind of novel alternative clean-out systems of ODS (Ozone Depleting Substances) leaning solvent.It is used widely in electronic industry, can be used for the cleaning to various CDs, liquid-crystal display, magnetic head, chip, circuit card base, module; Also can be used for the cleaning of optical lens, Printing screen, printing ink, metal.
Present homemade lactic acid ester can only be used for industries such as food as additive.The lactic acid by product that exists in the lactic acid ester is difficult to separate with lactic acid ester, and its color of lactic acid ester that distillation obtains can not satisfy request for utilization.Other impurity such as pyruvate also are difficult to separate through conventional distillation, also are difficult to solve through gac.Lactic acid ester can be brought the pollution of metals ion and nonmetallic ion in the preparation process, according to different preparation, reach as high as 500pm.And the lactic acid ester of electronic-grade needs unique high purity (mass content is more than 99.5%) and utmost point low-metal content (below the 10ppb) to satisfy semi-conductor industry to high-quality requirement.Thereby in practical application, quality of production height and stable lactic acid ester product are very important.
Given this, a kind of that lactic acid ester is carried out the new technology of ultra-pure purifying treatment is necessary in development.
Summary of the invention
The purpose of this invention is to provide a kind of purified lactic acid esters product; It is the new technology of methyl lactate, ethyl lactate and n-Butyl lactate; To obtain the electronic-grade lactate product of its ultra-high purity; Purity is higher than 99.9999%, and metal ion content is lower than 3ppb, can be semi-conductor industry high-quality solvent and clean-out system are provided.
For realizing above-mentioned target, technical scheme of the present invention is following:
A kind of production technique of electronic-grade lactic acid ester product, it by flash system-Tuo light and work in-process distillation system-activated carbon decolorizing system-ion exchange system form.Its flow process is as shown in Figure 1, and it may further comprise the steps:
The food grade lactate that (1) will contain 99.0% above purity of complicated impurity composition adds in the flasher; Through vacuum flashing operation, low-boiling-point substances such as contained part moisture content and alcohols will go out from the flasher evaporated on top with gaseous state in the raw material, after the evaporator overhead condenser condensation, discharge; Liquid phase material in the flasher is discharged from the flasher bottom; And being sent to the further rectifying separation of lightness-removing column, the working pressure of flasher is controlled at 5 ~ 100KPa, preferably 10 ~ 60KPa; Service temperature is 68 ~ 142 ℃, preferably 80 ~ 130 ℃;
The described lactate bullion of technology of the present invention is through the flasher operation, and purpose is to remove low-boiling-point substances such as 15 ~ 65% contained moisture content of lactate bullion and alcohols, and is excellent to remove 20 ~ 45% of low-boiling-point substance total amounts such as moisture content and alcohols.So both alleviate the processing load of lightness-removing column, dwindled the facility investment of lightness-removing column and annex thereof, can reduce the energy expenditure of whole process again significantly;
(2) lactate after the vacuum flashing gets into lightness-removing column; In lightness-removing column; Low-boiling-point substances such as remaining moisture content and alcohol almost all obtain removing in the material, and distillate from cat head, owing to wherein contain lactate; So it will be sent to flasher separations that circulate once more, the material that the light tower bottom of autospasy is discharged is then sent into treating tower and is further made with extra care;
Above-mentioned lightness-removing column is generally packing tower, or the combined column of packing tower and tray column, and material mainly is a stainless steel; In particular cases also can adopt pottery; Tetrafluoroethylene etc., theoretical plate number is 20 ~ 200, is preferably 30 ~ 120; Lightness-removing column cat head working pressure is 5 ~ 60KPa, preferably 10 ~ 40KPa; Service temperature is 34 ~ 102 ℃, preferably 50 ~ 90 ℃; The reflux ratio of lightness-removing column is 10 ~ 100, preferably 13 ~ 55;
(3) material rectifying in treating tower of lightness-removing column bottom discharge; Light constituents such as the water of remaining denier, alcohol in the cat head extraction material, and on the top of this tower rectifying section the lactate work in-process (its purity is more than 99.99992%) of side line extraction ultra-high purity.The lactate work in-process of this ultra-high purity are then sent to the activated carbon decolorizing system and are further handled;
From treating tower bottom extraction then is a small amount of lactate and lactic acid; And by the lactate bullion bring into by various impurity that are not vaporized removal such as spissated whole high boiling material, solid substance, mechanical impuritys; It will discharge and deliver to the harvesting of raffinate storage tank by the tower still, and concentrate and handle;
Described treating tower generally also is a packing tower, or the combined column of packing tower and tray column, and material mainly is a stainless steel; In particular cases also can adopt pottery; Tetrafluoroethylene etc., theoretical plate number is 30 ~ 200, is preferably 40 ~ 150; Treating tower cat head working pressure is 5 ~ 60KPa, preferably 10 ~ 40KPa; Service temperature is 70 ~ 137 ℃, preferably 80 ~ 120 ℃; The reflux ratio of treating tower is 0.05 ~ 3.0, is preferably 0.3 ~ 1.5;
During the lactate work in-process of treating tower top side line extraction ultra-high purity, but but both also liquid phase of vapour phase of extraction mode is excellent with the liquid phase extraction, the extraction position is 5 ~ 20 apart from the theoretical plate number of cat head, preferably 6 ~ 15;
(4) the lactate work in-process of the ultra-high purity of side line extraction on treating tower top get into the activated carbon decolorizing system, to remove pigment impurity or other impurity component wherein, make the colourity of product reach requirement.Used gac is preferably cocoanut active charcoal, or other specific surface area is equivalent to 1000-3000m
2The gac of/g;
(5) the lactate work in-process of the ultra-high purity after the process decolouring; Get into ion exchange system again; Remove positively charged ion (metals ion etc.) and negatively charged ion (cl ions etc.) respectively, or the neutral impurity of other metal ion, in ion exchange system; The neutral impurity of metals ion in the material and cl ions and other metal ion etc. obtains removing basically, and ion exchange system is a system that is made up of positively charged ion, negatively charged ion and non-cloudy non-cationic exchange column; Described three ion exchange columns are loaded Amberlite IR120 Na type Zeo-karb, Amberlite IRA402 Cl type anionite-exchange resin and Amberlite respectively
TMIon exchange resin and polymeric adsorbent that XAD4 type macroporous adsorbent resin or other performance are suitable with it; At last, by the lactate product of ion exchange system output be that purity is higher than more than 99.9999%, metal ion content is lower than 3ppb, colourless electronic-grade lactate product.
Above-mentioned production technique; Raw material storage tank in process of production and product storage tank need inflated with nitrogen to protect, and all devices good seal must not leak gas when negative-pressure operation; Necessary first pickling before the equipment internal surface feeds intake after manufacturing processed and installation finish and produces; Alkali cleaning, after high-purity washing (removing the water of zwitterion), for use behind the hot-air dry of cleaning again.
Above-mentioned production technique, production plant needs dust-free workshop, through GMP design and authentication; Finished product is through dustless filling and sealing and storage.
The production technique and the device of electronic-grade lactic acid ester product of the present invention; Food grade or other suitable other lactate of level of purity with 99.0% above purity are raw material; Can obtain purity and be higher than 99.9999%, metal ion content is lower than the electronic-grade lactate of 3ppb and colourless (≤No. 5 colour codes).
Characteristics of the present invention are to adopt integrated technologies such as flash distillation-two tower rectifying-activated carbon decolorizing-IX and dustless can storage, the lactic acid ester product of production ultra-high purity (like electronic-grade).The omnidistance recovery of lactate is greater than 98%.The purity of lactate is up to more than 99.9999%, and metal ion content is lower than 3ppb, and is colourless.Can satisfy the high request of electronic industry fully.Light constituent in the flow process of the present invention is got back to flasher and is handled again, and the second tower weight component focuses on, and has improved product yield significantly, has reduced the residue quantity discharged, has improved the economy and the processing cost of process.
Description of drawings
Fig. 1 is the technological process of production synoptic diagram of a kind of electronic-grade lactic acid ester product of the present invention, wherein: the 1-flasher; The 2-lightness-removing column; The 3-treating tower; 4,11,13 waste liquid outlets; 5,6,7-holding tank; 8,9,10-condensing surface; 12,15-tower bottom reboiler; 14-high-pure lactic acid ester work in-process extraction mouth; The outlet of 16-residue; The 17-decolorizing column; The 18-cationic exchange coloum; The 19-anion-exchange column; The non-cloudy non-cationic exchange column of 20-; The ultra-pure lactate products export of 21-.
Embodiment
Through embodiment the present invention is specifically described below, but can not be interpreted as restriction scope of patent protection of the present invention.
Embodiment 1
(1) the methyl lactate bullion is sent into flasher with the speed of 150kg/h; Wherein containing methyl alcohol is 4200 mg/kg, and water is 3060 mg/kg, and lactic acid is 1290 mg/kg; The methyl lactate mass content is 99.1%, and metals ion and heavy component foreign matter content are 450 mg/kg.The working pressure of flasher is 10KPa, and service temperature is about 84 ℃.In flasher, low-boiling-point substances such as about 65% moisture content and methyl alcohol are able to remove in the methyl lactate bullion.The solution of flasher bottom with the 118.95kg/h flow through being pumped into the lightness-removing column middle part.The structured packing of SS304 Stainless Steel Cloth is housed in the lightness-removing column, and number of theoretical plate is 92, and the tower internal diameter is 0.13m, and the cat head working pressure is 10KPa, and temperature is about 46 ℃.Low-boiling-point substance such as moisture content and methyl alcohol distillates from cat head, and reflux ratio is 25.0.Methyl lactate, heavy component etc. are discharged from the lightness-removing column still with the 118.45kg/h flow, through being pumped to the opening for feed of treating tower.
(2) the treating tower internals adopt the structured packing of SS316L Stainless Steel Cloth, and number of theoretical plate is 135, and the tower internal diameter is 0.30m, and the cat head working pressure is 10KPa, and temperature is 87 ℃.The top extraction of treating tower contains the methyl lactate of low-boiling-point substances such as trace water and methyl alcohol, is sent to the flasher circulation and separates, and operating reflux ratio is 3.0.The methyl lactate of ultra-high purity (mass content is 99.999956%) is sent to the decolouring of activated carbon decolorizing system again with the side line liquid phase extraction from tower top of 118.02kg/h flow (extraction mouth position is 16 apart from the theoretical plate number of cat head).The activated carbon decolorizing system is the fixed bed decolorizing column, and post is high 2 meters, and gac is loaded and highly is 1.6 meters, 0.5 meter of diameter.Gac is a coconut husk type gac, and specific surface area is 2800m
2/ g.After decolouring, material is colourless liquid (≤No. 5 colour code).
Afterwards; Material is sent to ion exchange system again; Respectively after yin, yang, non-cloudy non-cationic exchange resin are handled, (wherein water content is lower than 3.5mg/kg, and methanol content is lower than 1.4mg/kg can to obtain electronic-grade methyl lactate product more than 99.999981%; Lactic acid content is lower than 7.6 mg/kg, and metal ion content is lower than 2.5 μ g/kg).The post height of yin, yang, non-cloudy non-cationic exchange column is 2 meters, and diameter is 0.53 meter, and the resin of filling respectively is Amberlite IR120 Na type Zeo-karb, Amberlite IRA402 Cl type anionite-exchange resin and Amberlite
TMXAD4 type macroporous adsorbent resin.
The still raffinate is then discharged from the tower still with the 0.43kg/h flow, and is admitted to the raffinate storage tank and waits to run up to and focus on after a certain amount of.
Specification product then are admitted to the product storage tank of nitrogen envelope, and when outward transport, load and transport behind dustless filling and sealing through automatic filling machine.
Embodiment 2
(1) the ethyl lactate bullion is sent into flasher with the speed of 100kg/h; Wherein containing ethanol is 3070mg/kg, and water is 2130mg/kg, and lactic acid is 1420mg/kg; The ethyl lactate mass content is 99.3%, and metals ion and heavy component foreign matter content are 380mg/kg.The working pressure of flasher is 5KPa, and service temperature is about 68 ℃.Low-boiling-point substances such as the moisture content of about 15% in the ethyl lactate bullion and ethanol are able to remove.The solution of flasher bottom with the 91.41kg/h flow through being pumped into the lightness-removing column middle part.The structured packing of SS304 Stainless Steel Cloth is housed in the lightness-removing column, and number of theoretical plate is 20, and the tower internal diameter is 0.1m, and the cat head working pressure is 5KPa, and temperature is about 34 ℃.Low-boiling-point substance such as moisture content and ethanol distillates from cat head, and reflux ratio is 75.0.Ethyl lactate and heavy component etc. are discharged from the lightness-removing column still with the 90.91kg/h flow, through being pumped to the opening for feed of treating tower.
(2) the treating tower column internals adopts the structured packing of SS316L Stainless Steel Cloth, and number of theoretical plate is 30, and the tower internal diameter is 0.26m, and the cat head working pressure is 5KPa, and temperature is 70 ℃.The top extraction of treating tower contains the ethyl lactate of low-boiling-point substances such as small amount of moisture and ethanol, is sent to the flasher circulation and separates, and operating reflux ratio is 0.8.The ethyl lactate of ultra-high purity (mass content is 99.99994%) is sent to the decolouring of activated carbon decolorizing system again with the side line liquid phase extraction from tower top of 90.40kg/h flow (extraction mouth position is 5 apart from the theoretical plate number of cat head).The activated carbon decolorizing system is the fixed bed decolorizing column, and post is high 2 meters, and gac is loaded and highly is 1.6 meters, 0.41 meter of diameter.Gac is a coconut husk type gac, and specific surface area is 2800m
2/ g.After decolouring, material is colourless liquid (≤No. 5 colour code).
Afterwards; Material is sent to ion exchange system again; Respectively after yin, yang, non-cloudy non-cationic exchange resin are handled, (wherein water content is lower than 30.3mg/kg, and ethanol content is lower than 10.1 mg/kg can to obtain electronic-grade ethyl lactate product more than 99.999950%; Lactic acid content is lower than 5.1 mg/kg, and metal ion content is lower than 2.7 μ g/kg).The post height of yin, yang, non-cloudy non-cationic exchange column is 2 meters, and diameter is 0.43 meter, and the resin of filling is respectively Amberlite IR120 Na type Zeo-karb, Amberlite IRA402 Cl type anionite-exchange resin and Amberlite
TMXAD4 type macroporous adsorbent resin.
The still raffinate is then discharged from the tower still with the 0.51kg/h flow, and is admitted to the raffinate storage tank and waits to run up to and focus on after a certain amount of.
Specification product then are admitted to the product storage tank of nitrogen envelope, and when outward transport, load and transport behind dustless filling and sealing through automatic filling machine.
Embodiment 3
(1) the methyl lactate bullion is sent into flasher with the speed of 1500kg/h; Wherein containing methyl alcohol is 2620 mg/kg, and water is 3170 mg/kg, and lactic acid is 2760 mg/kg; The methyl lactate mass content is 99.1%, and metals ion and heavy component foreign matter content are 450 mg/kg.The working pressure of flasher is 100KPa, and service temperature is about 142 ℃.Low-boiling-point substances such as the moisture content of about 33% in the methyl lactate bullion and methyl alcohol are able to remove.The solution of flasher bottom with the 1376.33kg/h flow through being pumped into the lightness-removing column middle part.The structured packing of SS304 Stainless Steel Cloth is housed in the lightness-removing column, and number of theoretical plate is 90, and the tower internal diameter is 0.37m, and the cat head working pressure is 10KPa, and temperature is 47 ℃.Low-boiling-point substance such as moisture content and methyl alcohol distillates from cat head, and reflux ratio is 55.0.Methyl lactate and heavy component etc. are discharged from the lightness-removing column still with the flow of 1366.33 kg/h, through being pumped to the opening for feed of treating tower.
(2) the treating tower internals adopt the structured packing of SS316L Stainless Steel Cloth, and number of theoretical plate is 160, and the tower internal diameter is 0.82m, and the cat head working pressure is 10KPa, and temperature is 87 ℃.The top extraction of treating tower contains the methyl lactate of low-boiling-point substances such as small amount of moisture and methyl alcohol, is sent to the flasher circulation and separates, and operating reflux ratio is 0.05.The ethyl lactate of ultra-high purity (mass content is 99.999937%) is sent to the decolouring of activated carbon decolorizing system again with the side line liquid phase extraction from tower top of 1360.21kg/h flow (extraction mouth position is 12 apart from the theoretical plate number of cat head).The activated carbon decolorizing system is the fixed bed decolorizing column, and post is high 4 meters, and gac is loaded and highly is 3.2 meters, 1.5 meters of diameters.Gac is a coconut husk type gac, and specific surface area is 2800m
2/ g.After decolouring, material is colourless liquid (≤No. 5 colour code).
Afterwards; Material is sent to ion exchange system again; Respectively after yin, yang, non-cloudy non-cationic exchange resin are handled, (wherein water content is lower than 31mg/kg, and ethanol content is lower than 10 mg/kg can to obtain electronic-grade ethyl lactate product more than 99.999943%; Lactic acid content is lower than 16 mg/kg, and metal ion content is lower than 1.9 μ g/kg).The post height of yin, yang, non-cloudy non-cationic exchange column is 4 meters, and diameter is 1.5 meters, and the resin of filling is respectively Amberlite IR120 Na type Zeo-karb, Amberlite IRA402 Cl type anionite-exchange resin and Amberlite
TMXAD4 type macroporous adsorbent resin.
The still raffinate is then discharged from the tower still with the 6.12kg/h flow, and is admitted to the raffinate storage tank and waits to run up to and focus on after a certain amount of.
Specification product then are admitted to the product storage tank of nitrogen envelope, and when outward transport, load and transport behind dustless filling and sealing through automatic filling machine.
Embodiment 4
(1) the n-Butyl lactate bullion is sent into flasher with the speed of 1500kg/h; Wherein containing butanols is 3120 mg/kg, and water is 1880 mg/kg, and lactic acid is 2510 mg/kg; The n-Butyl lactate mass content is 99.1%, and metals ion and heavy component foreign matter content are 1490 mg/kg.The working pressure of flasher is 23.5KPa, and service temperature is about 108 ℃.Low-boiling-point substances such as the moisture content of about 30% in the n-Butyl lactate bullion and butanols are able to remove.The solution of flasher bottom with the 1372.74kg/h flow through being pumped into the lightness-removing column middle part.The structured packing of SS304 Stainless Steel Cloth is housed in the lightness-removing column, and number of theoretical plate is 200, and the tower internal diameter is 0.53m, and the cat head working pressure is 24KPa, and temperature is about 69 ℃.Low-boiling-point substance such as moisture content and butanols distillates from cat head, and reflux ratio is 100.0.N-Butyl lactate and heavy component etc. are discharged from the lightness-removing column still with the 1356.74kg/h flow, through being pumped to the opening for feed of treating tower.
(2) the treating tower column internals adopts the structured packing of SS316L Stainless Steel Cloth, and number of theoretical plate is 200, and the tower internal diameter is 0.81m, and the cat head working pressure is 25KPa, and temperature is 111 ℃.The top extraction of treating tower contains low-boiling-point substance n-Butyl lactates such as small amount of moisture and butanols, is sent to the flasher circulation and separates, and operating reflux ratio is 0.5.
The n-Butyl lactate of ultra-high purity (mass content is 99.999926%) is sent to the decolouring of activated carbon decolorizing system again with the side line liquid phase extraction from tower top of 1350.1kg/h flow (extraction mouth position is 20 apart from the theoretical plate number of cat head).The activated carbon decolorizing system is the fixed bed decolorizing column, and post is high 4 meters, and gac is loaded and highly is 3.2 meters, 1.5 meters of diameters.Gac is a coconut husk type gac, and specific surface area is 2800m
2/ g.After decolouring, material is colourless liquid (≤No. 5 colour code).
Afterwards; Material is sent to ion exchange system again; Respectively after yin, yang, non-cloudy non-cationic exchange resin are handled, (wherein water content is lower than 1mg/kg, and butanol content is lower than 53.7 mg/kg can to obtain electronic-grade n-Butyl lactate product more than 99.999941%; Lactic acid content is lower than 3 mg/kg, and metal ion content is lower than 2.3 μ g/kg).The post height of yin, yang, non-cloudy non-cationic exchange column is 4 meters, and diameter is 1.5 meters, and the resin of filling is respectively Amberlite IR120 Na type Zeo-karb, Amberlite IRA402 Cl type anionite-exchange resin and Amberlite
TMXAD4 type macroporous adsorbent resin.
The still raffinate is then discharged from the tower still with the 6.74kg/h flow, and is admitted to the raffinate storage tank and waits to run up to and focus on after a certain amount of.
Specification product then are admitted to the product storage tank of nitrogen envelope, and when outward transport, load and transport behind dustless filling and sealing through automatic filling machine.
Embodiment 5
(1) the n-Butyl lactate bullion is sent into flasher with the speed of 150kg/h; Wherein containing butanols is 2970mg/kg, and water is 2870mg/kg, and lactic acid is 3470mg/kg; The n-Butyl lactate mass content is 99.0%, and metals ion and heavy component foreign matter content are 430mg/kg.The working pressure of flasher is 24KPa, and service temperature is about 108 ℃.Low-boiling-point substances such as the moisture content of about 31% in the n-Butyl lactate bullion and butanols are able to remove.The solution of flasher bottom with the 136.14kg/h flow through being pumped into the lightness-removing column middle part.The structured packing of SS304 Stainless Steel Cloth is housed in the lightness-removing column, and number of theoretical plate is 150, and the tower internal diameter is 0.15m, and the cat head working pressure is 25KPa, and temperature is 111 ℃.Low-boiling-point substance such as moisture content and butanols distillates from cat head, and reflux ratio is 50.0.N-Butyl lactate and heavy component etc. are discharged from the lightness-removing column still with the 135.15kg/h flow, through being pumped to the opening for feed of treating tower.
(2) the treating tower column internals adopts the structured packing of SS316L Stainless Steel Cloth, and number of theoretical plate is 120, and the tower internal diameter is 0.26m, and the cat head working pressure is 25KPa, and temperature is 111 ℃.The top extraction of treating tower contains low-boiling-point substance ethyl lactates such as small amount of moisture and butanols, is sent to the flasher circulation and separates, and operating reflux ratio is 0.5.The n-Butyl lactate of ultra-high purity (mass content is 99.999946%) is sent to the decolouring of activated carbon decolorizing system again with the side line liquid phase extraction from tower top of 134.12kg/h flow (extraction mouth position is 12 apart from the theoretical plate number of cat head).The activated carbon decolorizing system is the fixed bed decolorizing column, and post is high 2 meters, and gac is loaded and highly is 1.6 meters, 0.5 meter of diameter.Gac is a coconut husk type gac, and specific surface area is 2800m
2/ g.After decolouring, material is colourless liquid (≤No. 5 colour code).
Afterwards; Material is sent to ion exchange system again; Respectively after yin, yang, non-cloudy non-cationic exchange resin are handled, (wherein water content is lower than 1mg/kg, and butanol content is lower than 23.3 mg/kg can to obtain electronic-grade n-Butyl lactate product more than 99.999970%; Lactic acid content is lower than 2 mg/kg, and metal ion content is lower than 1.5 μ g/kg).The post height of yin, yang, non-cloudy non-cationic exchange column is 2 meters, and diameter is 0.5 meter, and the resin of filling is respectively Amberlite IR120 Na type Zeo-karb, Amberlite IRA402 Cl type anionite-exchange resin and Amberlite
TMXAD4 type macroporous adsorbent resin.
The still raffinate is then discharged from the tower still with the 1.03kg/h flow, and is admitted to the raffinate storage tank and waits to run up to and focus on after a certain amount of.
Specification product then are admitted to the product storage tank of nitrogen envelope, and when outward transport, load and transport behind dustless filling and sealing through automatic filling machine.
Embodiment 6
(1) the ethyl lactate bullion is sent into flasher with the speed of 1500kg/h; Wherein contain ethanol 3130 mg/kg, water is 1970 mg/kg, and lactic acid is 2020 mg/kg; The ethyl lactate mass content is 99.2%, and metals ion and heavy component foreign matter content are 980 mg/kg.The working pressure of flasher is 68KPa, and service temperature is about 140 ℃.Low-boiling-point substances such as the moisture content of about 65% in the ethyl lactate bullion and ethanol are able to remove.The solution of flasher bottom with the 1173.41kg/h flow through being pumped into the lightness-removing column middle part.The structured packing of SS304 Stainless Steel Cloth is housed in the lightness-removing column, and number of theoretical plate is 30, and the tower internal diameter is 0.13m, and the cat head working pressure is 60KPa, and temperature is about 102 ℃.Low-boiling-point substance such as moisture content and ethanol distillates from cat head, and reflux ratio is 10.0.Ethyl lactate and heavy component etc. are discharged from the lightness-removing column still with the 1153.40kg/h flow, through being pumped to the opening for feed of treating tower.
(2) the treating tower column internals adopts the structured packing of SS316L Stainless Steel Cloth, and number of theoretical plate is 150, and the tower internal diameter is 0.33m, and the cat head working pressure is 60KPa, and temperature is 137 ℃.The top extraction of treating tower contains low-boiling-point substance ethyl lactates such as small amount of moisture and ethanol, is sent to the flasher circulation and separates, and operating reflux ratio is 3.0.The ethyl lactate of ultra-high purity (mass content is 99.999938%) is sent to the decolouring of activated carbon decolorizing system again with the side line liquid phase extraction from tower top of 1145.40kg/h flow (extraction mouth position is 15 apart from the theoretical plate number of cat head).The activated carbon decolorizing system is the fixed bed decolorizing column, and post is high 4 meters, and gac is loaded and highly is 3.2 meters, 1.5 meters of diameters.Gac is a coconut husk type gac, and specific surface area is 2800m
2/ g.After decolouring, material is colourless liquid (≤No. 5 colour code).
Afterwards; Material is sent to ion exchange system again; Respectively after yin, yang, non-cloudy non-cationic exchange resin are handled, (wherein water content is lower than 19.3mg/kg, and ethanol content is lower than 7.8mg/kg can to obtain electronic-grade ethyl lactate product more than 99.999965%; Lactic acid content is lower than 4.7mg/kg, and metal ion content is lower than 2.4 μ g/kg).The post height of yin, yang, non-cloudy non-cationic exchange column is 4 meters, and diameter is 1.5 meters, and the resin of filling is respectively Amberlite IR120 Na type Zeo-karb, Amberlite IRA402 Cl type anionite-exchange resin and Amberlite
TMXAD4 type macroporous adsorbent resin.
The still raffinate is then discharged from the tower still with the 8.00kg/h flow, and is admitted to the raffinate storage tank and waits to run up to and focus on after a certain amount of.
Specification product then are admitted to the product storage tank of nitrogen envelope, and when outward transport, load and transport behind dustless filling and sealing through automatic filling machine.
Claims (6)
1. the production technique of an electronic-grade lactic acid ester product is characterized in that it may further comprise the steps:
Step 1. adds food grade or other suitable other lactate of level (hereinafter to be referred as the lactate bullion) of purity of 99.0% above purity in the flasher (1); Operate through vacuum flashing; Low-boiling-point substance such as contained 15% ~ 65% moisture content and alcohols will go out from flasher (1) evaporated on top with gaseous state in the solvent; After the evaporator overhead condenser condensation, discharge; Liquid phase material in the flasher (1) is discharged from flasher (1) bottom, and is sent to further processing of lightness-removing column (2), and the working pressure of flasher (1) is controlled at 5 ~ 100KPa; Service temperature is 68 ~ 142 ℃;
Step 2. is in lightness-removing column (2), and low-boiling-point substances such as remaining moisture content and alcohols obtain removing basically in the material, and distillate from cat head; Owing to wherein contain lactate,, send into then from the material of lightness-removing column (2) bottom discharge that treating tower (3) is further to be made with extra care so it is sent to flasher (1) separations that circulate once more; Described lightness-removing column (2) is a packing tower; Or the combined column of packing tower and tray column, theoretical plate number is 20 ~ 200, the cat head working pressure is 5 ~ 60KPa; The cat head service temperature is 34 ~ 102 ℃, and the trim the top of column ratio is 10.0 ~ 100.0;
Step 3. is in treating tower (3); The low-boiling-point substances such as denier moisture content and alcohol that remain in the material will be turned back in the flasher by extraction and circulation at cat head; Treating tower (3) but the lactate work in-process of then extraction ultra-high purity of top side line; The extraction position is 5 ~ 20 apart from the theoretical plate number of cat head, and it is sent to the activated carbon decolorizing system and further handles; The extraction of treating tower (3) bottom be a small amount of lactate with lactic acid and by the lactate bullion bring into by various impurity that are not vaporized removal such as spissated metals ion, whole high boiling material, solid substance, mechanical impuritys; Described treating tower (3) is a packing tower, or the combined column of packing tower and tray column, and theoretical plate number is 30 ~ 200, and the cat head working pressure is 5 ~ 60KPa, and the cat head service temperature is 70 ~ 137 ℃, and the trim the top of column ratio is 0.05 ~ 3.0;
The lactate work in-process of step 4. ultra-high purity of side line extraction on treating tower top; Prompt delivery deactivation carbon decoloring system (17) further handles; To remove pigment impurity or other impurity component wherein; Make the colourity of product reach requirement, used gac is a cocoanut active charcoal, or other specific surface area is equivalent to 1000-3000m
2The gac of/g;
Step 5. is through the lactate work in-process of the ultra-high purity after the decolouring; Get into ion exchange system again; Remove positively charged ion and negatively charged ion respectively; Or the neutral impurity of other metal ion; At last, by the lactate product of ion exchange system output be that purity is higher than more than 99.9999%, metal ion content is lower than 3ppb, colourless electronic-grade lactate product, described three ion exchange columns (18,19 and 20) are loaded Amberlite IR120 Na type Zeo-karb, Amberlite IRA402 Cl type anionite-exchange resin and AmberliteTM XAD4 type macroporous adsorbent resin respectively.
2. the production technique of electronic-grade lactic acid ester product according to claim 1 is characterized in that: the working pressure of the described flasher of step 1 (1) is 10 ~ 60KPa; Service temperature is 80 ~ 130 ℃.
3. the production technique of electronic-grade lactic acid ester product according to claim 1 is characterized in that: the theoretical plate number of the described lightness-removing column of step 2 is 30 ~ 120; Lightness-removing column cat head working pressure is 10 ~ 40KPa; Service temperature is 50 ~ 90 ℃; The reflux ratio of lightness-removing column is 0.3 ~ 1.5.
4. the production technique of electronic-grade lactic acid ester product according to claim 1 is characterized in that: the theoretical plate number of the described treating tower of step 3 is 40 ~ 150; Treating tower cat head working pressure is for being 10 ~ 40KPa; Service temperature is 80 ~ 120 ℃; The reflux ratio of treating tower is 0.3 ~ 1.5; The extraction position is 6 ~ 15 apart from the theoretical plate number of cat head.
5. the production technique of electronic-grade lactic acid ester product according to claim 1 is characterized in that: sepn process, comprise all storage tanks, and in nitrogen protection, adopt decompression operation; The all devices good seal must not leak gas when negative-pressure operation, necessary first pickling before the equipment internal surface feeds intake after manufacturing processed and installation finish and produces, and alkali cleaning, after high purity water cleans, for use behind the hot-air dry that cleans again.
6. the production technique of electronic-grade lactic acid ester product according to claim 1 is characterized in that: production plant is a dust-free workshop, through GMP design and authentication; Finished product is through dustless filling and sealing and storage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110277777.9A CN102381973B (en) | 2011-09-19 | 2011-09-19 | Production process of ultra-high purity (electronic grade) lactate product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110277777.9A CN102381973B (en) | 2011-09-19 | 2011-09-19 | Production process of ultra-high purity (electronic grade) lactate product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102381973A true CN102381973A (en) | 2012-03-21 |
| CN102381973B CN102381973B (en) | 2014-01-29 |
Family
ID=45821869
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110277777.9A Active CN102381973B (en) | 2011-09-19 | 2011-09-19 | Production process of ultra-high purity (electronic grade) lactate product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102381973B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610061A (en) * | 2015-02-06 | 2015-05-13 | 孝感市易生新材料有限公司 | Preparation method of electronic ethyl lactate |
| WO2017057320A1 (en) * | 2015-10-02 | 2017-04-06 | 三菱瓦斯化学株式会社 | High-purity carboxylic acid ester and method for producing same |
| CN113527093A (en) * | 2021-07-16 | 2021-10-22 | 东华工程科技股份有限公司 | System and method for preparing high-purity methyl lactate by direct esterification method |
| CN113603585A (en) * | 2021-09-23 | 2021-11-05 | 福州大学 | Continuous production process of ultra-pure methyl lactate |
| CN113979862A (en) * | 2021-10-14 | 2022-01-28 | 寿光金远东变性淀粉有限公司 | Method for continuously producing D-lactate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050096481A1 (en) * | 2001-10-05 | 2005-05-05 | Rainer Hildebrandt | Method for producing a hydroxyacid esters |
| CN1720215A (en) * | 2002-12-05 | 2006-01-11 | 阿肯马公司 | Continuous ethyl lactate preparation method |
| CN1723187A (en) * | 2002-12-05 | 2006-01-18 | 阿肯马公司 | Continuous method for preparing ethyl lactate |
-
2011
- 2011-09-19 CN CN201110277777.9A patent/CN102381973B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050096481A1 (en) * | 2001-10-05 | 2005-05-05 | Rainer Hildebrandt | Method for producing a hydroxyacid esters |
| CN1720215A (en) * | 2002-12-05 | 2006-01-11 | 阿肯马公司 | Continuous ethyl lactate preparation method |
| CN1723187A (en) * | 2002-12-05 | 2006-01-18 | 阿肯马公司 | Continuous method for preparing ethyl lactate |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610061A (en) * | 2015-02-06 | 2015-05-13 | 孝感市易生新材料有限公司 | Preparation method of electronic ethyl lactate |
| CN104610061B (en) * | 2015-02-06 | 2016-09-28 | 孝感市易生新材料有限公司 | The preparation method of electron level ethyl lactate |
| US20180273465A1 (en) * | 2015-10-02 | 2018-09-27 | Mitsubishi Gas Chemical Company, Inc. | High-purity carboxylic acid ester and method for producing same |
| KR20180059472A (en) * | 2015-10-02 | 2018-06-04 | 미츠비시 가스 가가쿠 가부시키가이샤 | High purity carboxylic acid esters and methods for their preparation |
| CN108137476A (en) * | 2015-10-02 | 2018-06-08 | 三菱瓦斯化学株式会社 | High-purity carboxylate and its manufacturing method |
| JPWO2017057320A1 (en) * | 2015-10-02 | 2018-07-19 | 三菱瓦斯化学株式会社 | High purity carboxylic acid ester and method for producing the same |
| WO2017057320A1 (en) * | 2015-10-02 | 2017-04-06 | 三菱瓦斯化学株式会社 | High-purity carboxylic acid ester and method for producing same |
| US20200002264A1 (en) * | 2015-10-02 | 2020-01-02 | Mitsubishi Gas Chemical Company, Inc. | High-purity carboxylic acid ester and method for producing same |
| TWI698425B (en) * | 2015-10-02 | 2020-07-11 | 日商三菱瓦斯化學股份有限公司 | Method for manufacturing high-purity carboxylic acid ester |
| US11046634B2 (en) * | 2015-10-02 | 2021-06-29 | Mitsubishi Gas Chemical Company, Inc. | High-purity carboxylic acid ester and method for producing same |
| KR102605799B1 (en) * | 2015-10-02 | 2023-11-23 | 미츠비시 가스 가가쿠 가부시키가이샤 | High purity carboxylic acid ester and method for producing the same |
| CN113527093A (en) * | 2021-07-16 | 2021-10-22 | 东华工程科技股份有限公司 | System and method for preparing high-purity methyl lactate by direct esterification method |
| CN113603585A (en) * | 2021-09-23 | 2021-11-05 | 福州大学 | Continuous production process of ultra-pure methyl lactate |
| CN113979862A (en) * | 2021-10-14 | 2022-01-28 | 寿光金远东变性淀粉有限公司 | Method for continuously producing D-lactate |
| CN113979862B (en) * | 2021-10-14 | 2024-02-13 | 寿光金远东变性淀粉有限公司 | Method for continuously producing D-lactate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102381973B (en) | 2014-01-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5185481A (en) | Method for the separation of impurities from crude ethanol aqueous solution | |
| CN102381973B (en) | Production process of ultra-high purity (electronic grade) lactate product | |
| US8628643B2 (en) | Process to remove product alcohol from a fermentation by vaporization under vacuum | |
| KR20090122284A (en) | Process for the manufacture of dichloropropanol | |
| KR20060090764A (en) | A method for the manufacture of carboxylic acid ester by means of a reactive distillation | |
| CN105439855A (en) | Refinement method and device for synthesizing ethyl acetate through esterification | |
| CN104109078B (en) | A kind of method that in Sulpyrine production, ethanol reclaims | |
| CN101709025B (en) | Compound cross-flow liquid-liquid extraction separation method of methylal-methanol azeotropic system | |
| CN110072805A (en) | Method for purifying the salt acid composition of pollution | |
| CN101074258B (en) | Method for separating and extracting phytosterin and Vitamin E from soyabean deodorization distillate | |
| CN102173991A (en) | Continuous alcohol-removing device and alcohol-removing method of di-sec-octyl phthalate | |
| CN1289448C (en) | Clean reclaiming process for byproduct chloromethane of glyphosate acid | |
| CN101823928B (en) | Clean production process for derivatives of para aminobenzoic acid by reactor coupled simulated moving bed | |
| CN1159231C (en) | Method and device for treating waste water containing acetic acid | |
| CN201990614U (en) | Continuous dealcoholizing device used for dicapryl phthalate | |
| EP3719008B1 (en) | Alkylene oxide production method and production system | |
| CN116253295A (en) | Preparation method of ultra-pure semiconductor grade sulfuric acid | |
| CN102229521B (en) | Process for refining crude glycerin and recovering byproducts | |
| EP2648818A1 (en) | A method for recovery of organic acid from dilute aqueous solution | |
| US8084651B2 (en) | Process for purification of glycerol | |
| CN101538188B (en) | Biodiesel byproduct crude glycerin refining method | |
| CN101544558B (en) | Method for obtaining high-purity methanoic acid from hydrous methanoic acid through separation and refining | |
| CN1288118C (en) | Clean reclaiming process for byproduct chloromethane of glyphosate acid | |
| CN103183610B (en) | A kind of method from low-purity methyl acetate high-purity methyl acetate | |
| CN102992930A (en) | Recovery process and separation device of toluene solvent in production process of alpha-acetyl-gamma butyrolactone |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |