CN107033000A - A kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly - Google Patents
A kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly Download PDFInfo
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- CN107033000A CN107033000A CN201610074787.5A CN201610074787A CN107033000A CN 107033000 A CN107033000 A CN 107033000A CN 201610074787 A CN201610074787 A CN 201610074787A CN 107033000 A CN107033000 A CN 107033000A
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- fixed bed
- lactate
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- continuous liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly, comprise the following steps：The low-carbon alcohols that the lactic acid and mass concentration for being 95% by mass concentration are 95% are sufficiently mixed in head tank, it is pumped into and is mounted with solid acid catalyst LC-51 or NKC-9 fixed bed reactors through charging, the solid catalytic esterification of liquid is carried out under the conditions of 70 ~ 90 DEG C of reaction temperature, 3 ~ 7h-1 of 0.1 ~ 0.3Mpa of reaction pressure and air speed.The present invention is improved traditional lactated reaction method, overcome equipment corrosion caused by liquid acid catalyst and sewage pollution environmental problem, introduce acid cation exchange resin catalyst, on the premise of rotational rate of lactic acid is ensured, batch esterification is improved to liquid and is catalyzed continuous esterification admittedly, operating condition is improved, improve equipment capacity, the mass fraction of lactate in production cycle, continuous catalytic reaction product is reduced 40 ~ 50%, the conversion ratio of lactic acid is more than 68%.
Description
Technical field
The present invention relates to a kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly, more particularly to a kind of method that continuous high-efficient prepares lactate.
Background technology
Lactate is mainly that lactic acid reacts obtained methyl lactate and ethyl lactate with low molecule alcohol dehydration esterification in the present invention, two kinds of lactates have the distinctive fragrance of esters, outward appearance is colourless transparent liquid, because its reaction raw materials is lactic acid, methanol or ethanol, so that two kinds of lactates have nontoxic and biodegradable performance, therefore in addition to as fine solvent, or a kind of important flavorant, with aroma type fragrance, for drinks and the additive of essence；In addition it is used as the lubricant and pharmaceutical intermediate of medicine in pharmaceuticals industry；It is used as important intermediate of flavouring agent and herbicide etc. in feed industry.
The synthetic method of lactate generally uses esterification process, i.e., by lactic acid and low-carbon alcohols, esterification is produced under bronsted acid catalyst effect, then obtains lactate product by vacuum batch distillation.Traditional production technology subject matter has at following 2 points：
（1）To improve the monomer conversion of lactic acid, continuous the water for reacting generation must be removed into reaction system, break the positive back reaction balance of esterification, and be used as often poisonous benzene and toluene of water entrainer etc.；（2）The concentrated sulfuric acid is widely used because of its high catalytic efficiency in traditional industry, but the concentrated sulfuric acid is serious to equipment corrosion, and subsequent treatment is complicated, cause technological process long, environmental pollution is big, and the concentrated sulfuric acid is used as liquid acid catalyst, it is unfavorable for successive reaction so that the production cycle is long, equipment capacity is low.
The content of the invention
It is an object of the invention to provide a kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly, to improve esterification rate, the production cycle is reduced, equipment capacity is improved, and then reduce production cost.
Technical scheme is summarized as follows：Admittedly catalysis prepares the method for lactate to a kind of continuous liquid of fixed bed, it is characterized in that comprising the following steps：The low-carbon alcohols that the lactic acid and mass concentration for being 95% first by mass concentration are 95% are sufficiently mixed in head tank, it is pumped into through charging in the fixed bed reactors for being mounted with solid acid catalyst, the solid catalytic esterification of liquid is carried out under certain reaction temperature, reaction pressure and residence-time conditions, products therefrom is then obtained into lactate crude product by batch fractionating.
Described low-carbon alcohols are methanol or ethanol.
Described lactic acid and the mol ratio of low-carbon alcohols are 1:2~1:4.
Described fixed bed reactor catalyst is large aperture acid cation exchange resin, model LC-51 or NKC-9.
The reaction temperature of described fixed bed reactors is 70 ~ 90 DEG C, and reaction pressure is 0.1 ~ 0.3Mpa.
3 ~ 7h-1 of air speed of described fixed bed reactors.
The present invention is improved traditional lactated reaction method, overcome equipment corrosion caused by liquid acid catalyst and sewage pollution environmental problem, introduce acid cation exchange resin catalyst, on the premise of rotational rate of lactic acid is ensured, batch esterification is improved to liquid and is catalyzed continuous esterification admittedly, operating condition is improved, improve equipment capacity, the mass fraction of lactate in production cycle, continuous catalytic reaction product is reduced 40 ~ 50%, the conversion ratio of lactic acid is more than 68%.
Embodiment
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
Admittedly catalysis prepares the method for lactate to a kind of continuous liquid of fixed bed, it is characterized in that comprising the following steps：
（1）It is 1 in molar ratio:The methanol that the lactic acid and mass fraction that mass fraction is 95% by 3 ratio are 95% is well mixed in head tank；（2）Squeezed into and be mounted with the fixed bed reactors of LC-51 type acid cation exchange resins by feed pump, controlling reaction temperature is 80 DEG C, and reaction pressure is 0.3Mpa, air speed 5h-1；（3）Gas chromatographic analysis is carried out to esterification reaction product, the mass fraction of methyl lactate is 45%, the conversion ratio of lactic acid is 73%.
Embodiment 2
Admittedly catalysis prepares the method for lactate to a kind of continuous liquid of fixed bed, it is characterized in that comprising the following steps：
（1）It is 1 in molar ratio:The ethanol that the lactic acid and mass fraction that mass fraction is 95% by 2 ratio are 95% is well mixed in head tank；（2）Squeezed into and be mounted with the fixed bed reactors of NKC-9 type acid cation exchange resins by feed pump, controlling reaction temperature is 70 DEG C, and reaction pressure is 0.2Mpa, air speed 4h-1；（3）Gas chromatographic analysis is carried out to esterification reaction product, the mass fraction of methyl lactate is 42%, the conversion ratio of lactic acid is 68%.
Claims (6)
1. catalysis prepares the method for lactate to a kind of continuous liquid of fixed bed admittedly, it is characterized in that comprising the following steps：The low-carbon alcohols that the lactic acid and mass concentration for being 95% by mass concentration are 95% are sufficiently mixed in head tank, it is pumped into through charging in the fixed bed reactors for being mounted with solid acid catalyst, the solid catalytic esterification of liquid is carried out under certain reaction temperature, reaction pressure and residence-time conditions.
2. the continuous liquid of a kind of fixed bed method that catalysis prepares lactate admittedly according to claim 1, it is characterised in that described low-carbon alcohols are methanol or ethanol.
3. the continuous liquid of a kind of fixed bed method that catalysis prepares lactate admittedly according to claim 1, it is characterised in that described lactic acid and the mol ratio of low-carbon alcohols are 1:2~1:4.
4. the continuous liquid of a kind of fixed bed method that catalysis prepares lactate admittedly according to claim 1, it is characterised in that described fixed bed reactors solid acid catalyst is large aperture acid cation exchange resin, model LC-51 or NKC-9.
5. the continuous liquid of a kind of fixed bed method that catalysis prepares lactate admittedly according to claim 1, it is characterised in that the reaction temperature of described fixed bed reactors is 70 ~ 90 DEG C, reaction pressure is 0.1 ~ 0.3Mpa.
6. a kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly according to claim 1, it is characterised in that 3 ~ 7h-1 of air speed of described fixed bed reactors.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610074787.5A CN107033000A (en) | 2016-02-03 | 2016-02-03 | A kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610074787.5A CN107033000A (en) | 2016-02-03 | 2016-02-03 | A kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107033000A true CN107033000A (en) | 2017-08-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610074787.5A Withdrawn CN107033000A (en) | 2016-02-03 | 2016-02-03 | A kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly |
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| CN (1) | CN107033000A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112588208A (en) * | 2020-12-22 | 2021-04-02 | 河南金丹乳酸科技股份有限公司 | Process for preparing ethyl lactate by catalytic esterification of fixed bed reactor |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102180A (en) * | 1993-10-28 | 1995-05-03 | 国营吴江香料厂 | New technology for producing ethyl lactate |
| WO2004052826A2 (en) * | 2002-12-05 | 2004-06-24 | Arkema | Continuous method for preparing ethyl lactate |
| CN101492367A (en) * | 2009-03-11 | 2009-07-29 | 合肥工业大学 | Method for fine purification of lactic acid |
-
2016
- 2016-02-03 CN CN201610074787.5A patent/CN107033000A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102180A (en) * | 1993-10-28 | 1995-05-03 | 国营吴江香料厂 | New technology for producing ethyl lactate |
| WO2004052826A2 (en) * | 2002-12-05 | 2004-06-24 | Arkema | Continuous method for preparing ethyl lactate |
| CN101492367A (en) * | 2009-03-11 | 2009-07-29 | 合肥工业大学 | Method for fine purification of lactic acid |
Non-Patent Citations (2)
| Title |
|---|
| 刘模等: ""阳离子交换树脂床催化乳酸与甲醇酯化工艺的优化"", 《精细化工》 * |
| 李进军等: "《绿色化学导论 第2版 INTRODUCTION TO GREEN CHEMISTRY》", 31 August 2015, 武汉大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112588208A (en) * | 2020-12-22 | 2021-04-02 | 河南金丹乳酸科技股份有限公司 | Process for preparing ethyl lactate by catalytic esterification of fixed bed reactor |
| 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 |
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Address after: 300384 Nankai District Alex Hua Tian Road, Tianjin international business center, No. 6020, No. 2 Applicant after: Tianjin Zhongfu environmental Polytron Technologies Inc Address before: 300384 Nankai District Alex Hua Tian Road, Tianjin international business center, No. 6020, No. 2 Applicant before: TIANJIN ZHONGFU ENGINEERING TECHNOLOGY CO., LTD. |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170811 |
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| WW01 | Invention patent application withdrawn after publication |