CN103724274A - Compound catalyst allantoin synthesis method - Google Patents
Compound catalyst allantoin synthesis method Download PDFInfo
- Publication number
- CN103724274A CN103724274A CN201310663368.1A CN201310663368A CN103724274A CN 103724274 A CN103724274 A CN 103724274A CN 201310663368 A CN201310663368 A CN 201310663368A CN 103724274 A CN103724274 A CN 103724274A
- Authority
- CN
- China
- Prior art keywords
- wallantoin
- synthetic method
- acid
- allantoin
- glyoxylic 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/66—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D233/88—Nitrogen atoms, e.g. allantoin
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention relates to a chemical product synthesis technique, in particular to a compound catalyst allantoin sysnthesis method, which comprises the steps as follows: adding a glyoxylic acid aqueous solution, urea, catalysts, methanol, sodium laurate accounted by 0.1-0.2 percent of the glyoxylic acid aqueous solution in a reactor, wherein the catalysts comprise diammonium phosphate and phosphomolybdic acid; agitating; heating to 66-68 DEG C; after the 4-8-hour reaction, cooling the reaction mixture to the a room temperature; performing filtration, washing, drying; obtaining the finished product. The compound catalyst allantoin synthesis method provided by the invention is high in the synthesis yield of allantoin, short in reaction time, meanwhile lowers the risk during the synthesis and the production cost, is easier to treat the waste liquid, efficient in the production environment production, and has a practical application value.
Description
Technical field
The present invention relates to chemical synthetic technology, be specifically related to a kind of composite catalyst wallantoin synthetic method.
Background technology
Wallantoin has Promote cell's growth, accelerating wound, sterilization pain relieving, the effects such as coordinate plant growth, be widely used in pharmaceutical industries, cosmetics additive and agriculture field etc., the huge market demand, because natural wallantoin yields poorly, cannot meet the need of market, existing wallantoin mainly relies on chemical synthesis process to make, wherein the most general synthetic method of application is urea oxoethanoic acid condensation method, this method relatively other synthetic method to have synthesis condition comparatively simple, productive rate is advantages of higher relatively, but, productive rate remains the principal element of restriction wallantoin scale operation, and in production process, the processing problem of waste is also most important, therefore, in the urgent need on original synthetic method basis, improve formula, improve productive rate, and the pollution of reduction to environment, realizing wallantoin high-efficiency environment friendly produces.
Summary of the invention
The object of the invention is to, a kind of composite catalyst wallantoin synthetic method is provided, to improve synthetic yield, to achieve these goals, the technical solution used in the present invention is as follows:
A kind of composite catalyst wallantoin synthetic method, this synthetic method is: to adding aqueous glyoxylic acid, urea and catalyzer, methyl alcohol in reactor, be equivalent to the sodium laurate of aqueous glyoxylic acid 0.1-0.2%, stir, be heated to 66 ℃-68 ℃; After reaction 4-8h, reaction mixture is cooled to room temperature, filters, wash, dry, obtain finished product.Described catalyzer is: primary ammonium phosphate, phospho-molybdic acid, the two mol ratio is 1:3-4.
The mass concentration of described aqueous glyoxylic acid is 40%-50%.
Described oxoethanoic acid and the mol ratio of urea are 1:2.5-4, and the mol ratio of preferred oxoethanoic acid and urea is 1:3-3.5.
The mol ratio of described oxoethanoic acid and catalyzer is 1:0.03-0.05.
Described methanol usage is 1-2 times of aqueous glyoxylic acid volume.
Beneficial effect of the present invention is, improved catalyst formulation, the raw material relatively weak by acidity such as primary ammonium phosphate, phospho-molybdic acids replaced traditional strong acid catalyst, forms the wider buffered soln of acid range, not only reduced the danger in reaction process, reduced production cost, and together with the methyl alcohol adding, sodium laurate, improved wallantoin synthetic yield, shortened generated time, reduced the danger of waste liquid, production process environment-friendly high-efficiency.
Embodiment
Embodiment 1
The wallantoin of the present embodiment is synthesized by following methods: to adding aqueous glyoxylic acid, urea and catalyzer, methyl alcohol in reactor, be equivalent to the sodium laurate of aqueous glyoxylic acid 0.2%, stir, be heated to 66 ℃-68 ℃; After reaction 5h, reaction mixture is cooled to room temperature, filter, wash, dry, obtain finished product, wherein the mass concentration of aqueous glyoxylic acid is 50%, the mol ratio of oxoethanoic acid and urea is 1:2.5, catalyzer is: primary ammonium phosphate, phospho-molybdic acid, and primary ammonium phosphate, phospho-molybdic acid, the two mol ratio is 1:3-4.The mol ratio of oxoethanoic acid and catalyzer is 1:0.05, and methanol usage is 2 times of aqueous glyoxylic acid volume.
It is 60.7% that analysis obtains this embodiment synthetic allantoin productive rate.
Claims (5)
1. a composite catalyst wallantoin synthetic method, this synthetic method is: to adding aqueous glyoxylic acid, urea and catalyzer, methyl alcohol in reactor, be equivalent to the sodium laurate of aqueous glyoxylic acid 0.1-0.2%, stir, be heated to 66 ℃-68 ℃; After reaction 4-8h, reaction mixture is cooled to room temperature, filters, wash, dry, obtain finished product; Described catalyzer is: primary ammonium phosphate, phospho-molybdic acid, the two mol ratio is 1:3-4.
2. a kind of composite catalyst wallantoin synthetic method as claimed in claim 1, is characterized in that, the mass concentration of described aqueous glyoxylic acid is 40%-50%.
3. a kind of composite catalyst wallantoin synthetic method as claimed in claim 1, is characterized in that, the mol ratio of oxoethanoic acid and urea is 1:2.5-4, and the mol ratio of preferred oxoethanoic acid and urea is 1:3-3.5.
4. a kind of composite catalyst wallantoin synthetic method as claimed in claim 1, is characterized in that, the mol ratio of described oxoethanoic acid and catalyzer is 1:0.03-0.05.
5. a kind of composite catalyst wallantoin synthetic method as claimed in claim 1, is characterized in that, described methanol usage is 1-2 times of aqueous glyoxylic acid volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310663368.1A CN103724274A (en) | 2013-12-10 | 2013-12-10 | Compound catalyst allantoin synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310663368.1A CN103724274A (en) | 2013-12-10 | 2013-12-10 | Compound catalyst allantoin synthesis method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103724274A true CN103724274A (en) | 2014-04-16 |
Family
ID=50448608
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310663368.1A Pending CN103724274A (en) | 2013-12-10 | 2013-12-10 | Compound catalyst allantoin synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103724274A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190654A (en) * | 1998-02-16 | 1998-08-19 | 张永正 | Process of one-stage synthesizing allantoin from oxaldehyde |
| CN1296946A (en) * | 1999-11-18 | 2001-05-30 | 贺楚华 | Process for synthesizing allantoin |
| CN1528749A (en) * | 2003-09-29 | 2004-09-15 | 宁夏大学 | Allantoin synthesizing process |
| CN102010372A (en) * | 2010-11-22 | 2011-04-13 | 天津市职业大学 | Method for synthesizing allantoin by catalysis of phosphorous acid |
| CN102617476A (en) * | 2012-03-09 | 2012-08-01 | 北京桑普生物化学技术有限公司 | Method for synthesizing allantoin |
| CN102898376A (en) * | 2012-10-08 | 2013-01-30 | 北京桑普生物化学技术有限公司 | Allantoin synthesis method |
-
2013
- 2013-12-10 CN CN201310663368.1A patent/CN103724274A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190654A (en) * | 1998-02-16 | 1998-08-19 | 张永正 | Process of one-stage synthesizing allantoin from oxaldehyde |
| CN1296946A (en) * | 1999-11-18 | 2001-05-30 | 贺楚华 | Process for synthesizing allantoin |
| CN1528749A (en) * | 2003-09-29 | 2004-09-15 | 宁夏大学 | Allantoin synthesizing process |
| CN102010372A (en) * | 2010-11-22 | 2011-04-13 | 天津市职业大学 | Method for synthesizing allantoin by catalysis of phosphorous acid |
| CN102617476A (en) * | 2012-03-09 | 2012-08-01 | 北京桑普生物化学技术有限公司 | Method for synthesizing allantoin |
| CN102898376A (en) * | 2012-10-08 | 2013-01-30 | 北京桑普生物化学技术有限公司 | Allantoin synthesis method |
Non-Patent Citations (2)
| Title |
|---|
| 崔志敏等: "混酸H7PW12O42/H3PO4催化合成尿囊素的研究", 《郑州工程学院学报》, vol. 23, no. 2, 31 January 2002 (2002-01-31) * |
| 谢茹胜: "尿囊素的合成新法研究", 《海峡药学》, vol. 22, no. 8, 31 December 2010 (2010-12-31), pages 243 - 246 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102898376B (en) | Allantoin synthesis method | |
| CN102617476B (en) | Method for synthesizing allantoin | |
| CN1765888A (en) | Allantoin synthesis process | |
| SG156574A1 (en) | Method for regenerating catalyst for the production of methacrylic acid and process for preparing methacrylic acid | |
| CN101773840B (en) | Method for hydrothermal synthesis of carbon-silicon composite solid acid catalyst | |
| US20120095261A1 (en) | Process for preparation of alpha-ketoglutaric acid | |
| CN105541657A (en) | Method for preparing adipic acid dihydrazide | |
| CN105541588A (en) | Synthesis method of butanedione | |
| CN103145621A (en) | Allantoin preparation method | |
| CN103864618A (en) | Synthetic process of 1, 1-cyclopropane dicarboxylic acid dimethyl ester | |
| CN109206343A (en) | A kind of preparation method of adiponitrile | |
| CN103724274A (en) | Compound catalyst allantoin synthesis method | |
| CN104230708B (en) | A kind of preparation method of methyl-formiate | |
| CN103724272A (en) | Allantoin synthesis method | |
| CN101731628B (en) | Method for preparing casein peptide chelated iron | |
| CN102241654A (en) | Environmentally-friendly synthetic method of pyrimidine compound | |
| CN103724273A (en) | Allantoin synthesis method | |
| CN104248978B (en) | A kind of preparation method of phosphomolybdate crystal catalyst | |
| CN102503648A (en) | Method for producing ammonium phosphate sulfate by S-NPK (Sulfur-Containing Nitrogen-Phosphorus-Potassium Compounds) device | |
| CN102731250A (en) | Method for synthesizing sec-butyl alcohol | |
| CN101423465A (en) | Method for preparing anisic aldehyde by hydrogen peroxide oxidation of anethole through microwave aided acid catalysis | |
| CN105482126A (en) | Aldehyde group-terminated hyperbranched polymer leather retanning agent and preparation method thereof | |
| CN101973876B (en) | Synthesis method of acetylsalicylic acid | |
| CN101108365A (en) | Ferric trichloride modified ion exchange resin catalyzer, method of manufacturing the same and application thereof | |
| CN104030833A (en) | Chemical fertilizer for crops |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140416 |