CN1381436A - Process for synthesizing tartaric acid from maleic acid - Google Patents
Process for synthesizing tartaric acid from maleic acid Download PDFInfo
- Publication number
- CN1381436A CN1381436A CN 02119436 CN02119436A CN1381436A CN 1381436 A CN1381436 A CN 1381436A CN 02119436 CN02119436 CN 02119436 CN 02119436 A CN02119436 A CN 02119436A CN 1381436 A CN1381436 A CN 1381436A
- Authority
- CN
- China
- Prior art keywords
- molecular sieve
- mcm
- acid
- mesopore molecular
- maleic acid
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Catalysts (AREA)
Abstract
A process for synthesizing tartaria acid from maleic acid includes such steps as synthesizing mesoporous molecular sieve W-MCM-41, mixing it uniformly with maleic acid, 30% solution of hydrogen peroxide and water, reaction at 70 deg.C while stirring, then reflux, filtering to remove catalyst, adding concentrated sulfuric acid, thermal concentration, cooling to educe out crystal filtering, washing and drying to obtain the tartaric acid. Its advantages are recovery of catalyst, high purity, and no environmental pollution.
Description
Technical field
The present invention relates to a kind of tartaric synthetic method, specifically, the present invention synthesizes tartaric method with hydrogen peroxide and maleic acid as reactant.
Background technology
Tartrate is a kind of important organic raw material, and he is widely used as beverage and other acidification of food products agent, also is used for electroplating, making mirror, photograph, printing and dyeing, process hides, glass-ceramic, telecommunication apparatus, pharmacy etc.Tartrate mainly is present in various plants and the fruit with the form of sylvite, also has on a small quantity to exist with free state, and industrial glucose fermentation commonly used is produced Ltartaric acid.Existing tartrate is produced route and mainly contained two kinds of approach: (1) through wolframic acid catalysis, the hydrogen peroxide with 30% carries out epoxidation from MALEIC ANHYDRIDE, open loop and get [Japan Kokal7339,436 (1973) under acid then; Japan Kokal 7339,435 (1973)]; (2) maleic acid is under wolframic acid catalysis, and the high density hydrogen peroxide with 70% joins in the reaction system that is controlled at 0 ℃, carries out epoxidation, open loop under acid then (Ger.Offen 2,508,228 (1976)).These two kinds of approach respectively have drawback: tartrate can with multiple metal ion network and, when being Preparation of Catalyst tartrate with wolframic acid, product tartrate can't separate with wolframic acid, causes in the product W content too high, can not be used for food service industry and pharmaceutical industry.And first kind is raw material with the MALEIC ANHYDRIDE, and MALEIC ANHYDRIDE costs an arm and a leg, tartaric production cost increases, and second kind of approach need be with 70% high density hydrogen peroxide, and 70% hydrogen peroxide very easily decomposes, need keep in Dark Place, corrodibility is extremely strong, makes troubles to transportation.Particularly when 70% hydrogen peroxide joins in the system, must at first make whole system refrigeration to 0 ℃, this has increased the difficulty of industrialized production.
1992 is the discovery of the mesopore molecular sieve of representative with MCM41S, be catalysis, subjects such as separation and new inorganic material, opened up new research field. at the catalysis subject, with Ti, Zr, Mo, W etc. have the transition metal of certain catalytic activity, form with high dispersive embeds mesoporous molecular sieve framework, prepare novel mesopore molecular sieve catalytic material thus, and the macromolecular organic compound catalyzed conversion of carrying out on this basis research, be to develop very rapidly research field .W-MCM-41 in recent years at alkene epoxidation, the partial oxidation of arylamine, the hydroxylation of aromatic hydrocarbons, aspects such as the bis oxide hydroxylation of tetrahydrobenzene have excellent catalytic performance.
Summary of the invention
Purpose of the present invention provides a kind of tartaric synthetic method overcoming the deficiencies in the prior art.
The present invention makes the synthetic tartrate of catalyzer by mesopore molecular sieve W-MCM-41.Utilize maleic acid need not refrigeration, need not under the situation with 70% high density hydrogen peroxide as oxidant, lower concentration hydrogen peroxide as oxidant with 30% just can synthesize tartrate, and mesopore molecular sieve W-MCM-41 can with solution separating, greatly reduce tungsten to the tartaric pollution of product.
The tartaric method of preparation in turn includes the following steps among the present invention:
(1) maleic acid, mesopore molecular sieve W-MCM-41,30% superoxol and water are mixed,, reflux again in 70 ℃ of following stirring reactions;
(2) reaction solution cooling removes by filter mesopore molecular sieve;
(3) add the vitriol oil, ebuillition of heated concentrates;
(4) crystallization is separated out in cooling, filter, and washing, drying obtains tartrate.
The tungsten among the present invention among the used mesopore molecular sieve W-MCM-41 and the mol ratio of silicon are: 0.005-0.1: 1.
The consumption of the tartaric synthetic middle catalyzer mesopore molecular sieve W-MCM-41 that is provided among the present invention is: 0.01-1.0g/100ml.
Outstanding feature of the present invention is to be catalyzer with mesopore molecular sieve W-MCM-41, need not refrigeration, need not under the situation with 70% high density hydrogen peroxide as oxidant with maleic acid, lower concentration hydrogen peroxide as oxidant with 30% just can synthesize tartrate, and mesopore molecular sieve W-MCM-41 can separate with solution, thereby do not remain in the product tartrate, impure few in the product tartrate.Make the synthetic tartrate of catalyzer with wolframic acid and compare with traditional, the present invention has following several advantage: (1) reaction process need not refrigeration; (2) need not to make oxygenant with 70% high density hydrogen peroxide; (3) the tartaric productive rate of product is very high; (4) after epoxidation is finished, mesopore molecular sieve W-MCM-41 can separate with solution, thereby can reduce the tartaric pollution of product, make catalyzer institute synthetic product tartrate with wolframic acid and compare with traditional, W content significantly reduces (W content is 0.009%); (5) mesopore molecular sieve W-MCM-41 can reclaim and reuse, thereby is a kind of economy, eco-friendly synthetic method.
Embodiment
The invention will be further described below by embodiment:
Embodiment 1
Tartaric synthetic: as hydrogen peroxide and the 30ml water of 29.0g maleic acid, 0.5g mesopore molecular sieve W-MCM-41,60g30% to be mixed, react 8h, backflow 1h down at 70 ℃, cooling removes by filter mesopore molecular sieve, adds the 5.0ml vitriol oil, ebuillition of heated concentrates 2h, and crystallization is separated out in cooling, filter, washing, drying obtains product tartrate 35g, productive rate is 93%, fusing point 202-204 ℃.
Embodiment 2-4
According to method and the step of embodiment 1, but the consumption of change ammonium tungstate, the mole proportioning of each component is respectively in the precursor colloidal sol:
(2)0.005WO
3∶SiO
2
(3)0.010WO
3∶SiO
2
(4) 0.015WO
3: SiO
2(2) obtain the about 30g of product tartrate, productive rate about 80%, fusing point 202-204 ℃; (3) obtain the about 32g of product tartrate, productive rate about 85%, fusing point 202-204 ℃; (4) obtain the about 35g of product tartrate, productive rate about 93%, fusing point 202-204 ℃.
Embodiment 5
According to method and the step of embodiment 1, but the mesopore molecular sieve W-MCM-41 that catalyzer is reclaimed for embodiment 1.Obtain the about 30g of product tartrate, productive rate about 80%, fusing point 202-204 ℃.
Claims (3)
1. one kind from the synthetic tartaric method of maleic acid, it is characterized in that this method in turn includes the following steps:
(1) maleic acid, mesopore molecular sieve W-MCM-41,30% superoxol and water are mixed,, reflux again in 70 ℃ of following stirring reactions;
(2) reaction solution cooling removes by filter mesopore molecular sieve;
(3) add the vitriol oil, ebuillition of heated concentrates;
(4) crystallization is separated out in cooling, filter, and washing, drying obtains tartrate.
2. according to claims 1 described synthetic method, it is characterized in that the mol ratio of tungsten and silicon is 0.05-0.1 among the mesopore molecular sieve W-MCM-41: 1
3. according to claims 1 described synthetic method, it is characterized in that mesopore molecular sieve W-MCM-41 in consumption be 0.1-1.0g/100ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02119436 CN1131195C (en) | 2002-05-21 | 2002-05-21 | Process for synthesizing tartaric acid from maleic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02119436 CN1131195C (en) | 2002-05-21 | 2002-05-21 | Process for synthesizing tartaric acid from maleic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1381436A true CN1381436A (en) | 2002-11-27 |
| CN1131195C CN1131195C (en) | 2003-12-17 |
Family
ID=4744693
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02119436 Expired - Fee Related CN1131195C (en) | 2002-05-21 | 2002-05-21 | Process for synthesizing tartaric acid from maleic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1131195C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116393120A (en) * | 2023-03-31 | 2023-07-07 | 浙江大学 | Method and catalyst for preparing D, L-tartaric acid through microchannel reaction |
-
2002
- 2002-05-21 CN CN 02119436 patent/CN1131195C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116393120A (en) * | 2023-03-31 | 2023-07-07 | 浙江大学 | Method and catalyst for preparing D, L-tartaric acid through microchannel reaction |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1131195C (en) | 2003-12-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107803220B (en) | Supported imidazole ionic liquid catalyst and application thereof in preparation of cyclohexanone and cyclohexanol by catalytic oxidation of cyclohexane | |
| CN107983408A (en) | It is a kind of to prepare sulfoxide type catalyst and its selective method for preparing sulfoxide compound | |
| CN106006665A (en) | Method for preparing titanium silicalite molecular sieve TS-1 | |
| CN104923293A (en) | O-cresol isomerization catalyst, preparing method of o-cresol isomerization catalyst and method for catalyzed synthesis of mixture of m-cresol and p-cresol through o-cresol isomerization catalyst | |
| CN106380375B (en) | A kind of method of the continuous synthesizing adipic acid of micro passage reaction | |
| CN1131195C (en) | Process for synthesizing tartaric acid from maleic acid | |
| CN1131194C (en) | Process for preparing tartaric acid | |
| CN111548300A (en) | Synthesis process of phthalimide | |
| CN110498778B (en) | Method for preparing cyclohexene oxide by epoxidation of cyclohexene | |
| CN108276261B (en) | Method for preparing 2-bromofluorenone by catalyzing molecular oxygen oxidation in aqueous phase | |
| CN111747832B (en) | Method for preparing cyclohexanone | |
| CN113828352A (en) | Preparation method of supported palladium/titanium silicalite molecular sieve catalyst | |
| CN109569595B (en) | Catalytic system for preparing cyclohexene Ru through benzene selective hydrogenation, and preparation method and application thereof | |
| CN113755866B (en) | Preparation method of 2,4,6-tribromoaniline | |
| CN117186030A (en) | Preparation method of N-methylmorpholine-N-oxide | |
| CN117186031A (en) | Synthesis method of N-methylmorpholine-N-oxide | |
| CN114920787B (en) | Preparation method of fructose | |
| CN107602408A (en) | A kind of synthetic method of acetamino diethyl malonate | |
| CN116143139B (en) | FAU type molecular sieve synthesis method | |
| CN115246764B (en) | Clean production process of parachlorophenol | |
| CN113087644B (en) | Method for preparing 4-acetamino-benzene sulfinic acid | |
| CN115124413B (en) | Method for preparing hydroxycitronellal from hydroxycitronellol | |
| CN1305824C (en) | Method for preparing cyclohexanol and cyclohexanone by oxidizing cyclohexane | |
| CN116947062A (en) | Method for preparing titanium-silicon molecular sieve TS-1 from fluorine-containing silicon slag, modification and application thereof | |
| CN117816231A (en) | Catalyst for isomerisation of dichlorotoluene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |