CN105541726A - Allantoin production technology - Google Patents
Allantoin production technology Download PDFInfo
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- CN105541726A CN105541726A CN201610145032.XA CN201610145032A CN105541726A CN 105541726 A CN105541726 A CN 105541726A CN 201610145032 A CN201610145032 A CN 201610145032A CN 105541726 A CN105541726 A CN 105541726A
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- wallantoin
- urea
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- reaction mixture
- production technique
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an allantoin production technology. The technology comprises steps of feeding, reaction, filter-pressing and centrifugal washing, firstly, a glyoxylic acid aqueous solution, urea and a hydrogen peroxide catalyst are added to a reactor, stirred and heated, after the mixture reacts for a period, a certain amount of urea is added to the reactor, and the mixture is heated, stirred and reacts continuously; after the reaction, the reacted mixture is cooled and pumped into a filter press, compressed gas is introduced, solid-liquid separation of the reacted mixture is realized, and a filter cake and a filtrate are obtained; the filter cake is placed in a prefabricated mold, centrifugal dewater is performed on the basis, allantoin is washed after dewatering, and allantoin is washed with hot water and then washed with tap water; the filtrate is dried by an efficient centrifugal sprayer, and urea can be reduced to solids again after drying. The purity and the yield of the product are improved, the production cost is reduced, and clean production is realized.
Description
Technical field
The invention belongs to wallantoin production field, relate to a kind of wallantoin production technique.
Background technology
Wallantoin has Promote cell's growth, the effects such as accelerating wound, 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 obtain, wherein applying synthetic method the most general is urea, oxoethanoic acid condensation method, its reaction process is: feed intake-react-filter-dry-pulverize-detect-packaging-warehouse-in, it is comparatively simple that this method has synthesis condition relative to other synthetic method, productive rate is advantages of higher relatively, but, productive rate remains the principal element of restriction wallantoin scale operation, and the process problem of waste is also most important in production process, therefore, in the urgent need on original synthetic method basis, improve formula, improve productive rate, and the pollution reduced environment, realize wallantoin high-efficiency environment friendly to produce.
Existing wallantoin synthetic method is varied, its catalyzer added in synthesis procedure is also varied, but this operation introduces other ions a large amount of, cause the interference to synthetics reaction, have impact on reaction yield and purity, in addition, in prior art, urea waste is serious, cost improves, and is unfavorable for environmental protection.
Summary of the invention
The object of the present invention is to provide a kind of wallantoin production technique.
Object of the present invention can be achieved through the following technical solutions:
A kind of wallantoin production technique, this technique comprises: the reaction that feeds intake, press filtration and centrifuge washing step, first in reactor, add aqueous glyoxylic acid, urea and hydrogen peroxide catalyzed dose, stirring heating, after thing to be mixed reacts for some time, again in reactor, add a certain amount of urea, heat up to stir and continue reaction;
After having reacted, reaction mixture is cooled, then reaction mixture is pumped in pressure filter, pass into pressurized gas, make reaction mixture realize solid-liquid separation, obtain filter cake and filtrate respectively;
Above-mentioned filter cake is put into pre-formed, carries out centrifuge dehydration on this basis, and after dehydration, wallantoin washs, and first uses hot wash, and then with tap water; Above-mentioned filtrate is dry via efficient centrifugal spraying machine, and after dry, urea can be reduced into solid again.
By weight, mass concentration is aqueous glyoxylic acid 1-1.5 part of 53-66%, urea 5-7 part, hydrogen peroxide catalyzed dose of 0.1-0.15 part.
Described stirring heating temperature is 85-90 DEG C, and the reaction times is 3h, is again warming up to 95 DEG C, continues reaction 5h.
After having reacted, reaction mixture is cooled to 30 DEG C, then reaction mixture is pumped in pressure filter, pass into pressurized gas, press filtration under 2-4 standard atmospheric pressure effect, make reaction mixture realize solid-liquid separation.
Described centrifugal rotational speed 3500 turns/min, after dehydration, effective constituent Content of Allantoin can reach 95%; Washing 1h is carried out to the wallantoin obtained after centrifugal, first uses 30 DEG C of hot wash 20min during washing, and then use tap water.
Beneficial effect of the present invention: present invention process uses hydrogen peroxide catalyzed dose, does not introduce other ions, improves the purity of product; By by the excessive input of urea substep, improve the transformation efficiency of oxoethanoic acid, improve the yield of product; Utilize press filtration operation, make urea reuse to production process, reduce production cost, achieve cleaner production, accomplish the sustainable use of material; Product wallantoin first uses hot wash, and then with washing from the beginning, improves quality product greatly.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
A kind of wallantoin production technique, this technique produces wallantoin with urea and oxoethanoic acid generation condensation reaction, and processing step comprises: the reaction that feeds intake, press filtration and centrifuge washing operation;
Embodiment 1
First in reactor, add 1 part of mass concentration is the aqueous glyoxylic acid of 66%, 4 parts of urea and 0.1 part hydrogen peroxide catalyzed dose, stir and be heated to 85 DEG C, after thing reaction 3h to be mixed, again in reactor, adding 2 parts of urea, be warming up to 95 DEG C, stir and continue reaction 5h;
After having reacted, reaction mixture is cooled to 30 DEG C, then reaction mixture is pumped in pressure filter, pass into pressurized gas, press filtration under the pressure effect of pressurized gas (2-4 standard atmospheric pressure), makes reaction mixture realize solid-liquid separation, obtains filter cake and filtrate respectively;
The filter cake obtained puts into that prefabricated circular die is shaping, and filter cake is evenly distributed, consistency of thickness, carries out centrifuge dehydration on this basis, centrifugal rotational speed 3500 turns/min, and after dehydration, effective constituent Content of Allantoin can reach 95%; Washing 1h is carried out to the wallantoin obtained after centrifugal, first uses 30 DEG C of hot wash 20min during washing, and then use tap water.
The filtrate that above-mentioned press filtration is separated contains excessive urea and hydrogen peroxide catalyzed dose, this filtrate is dry via efficient centrifugal spraying machine, drying temperature is 200 DEG C, after dry, urea can be reduced into solid again, as raw materials for production reuse, peroxide decomposition becomes gas, not only reduces production cost, realize cleaner production, accomplish the sustainable use of material.
Embodiment 2
First in reactor, add 1.5 parts of mass concentrations is the aqueous glyoxylic acid of 53%, 5 parts of urea and 0.15 part hydrogen peroxide catalyzed dose, stir and be heated to 90 DEG C, after thing reaction 5h to be mixed, again in reactor, adding 1 part of urea, be warming up to 95 DEG C, stir and continue reaction 3h;
After having reacted, reaction mixture is cooled to 35 DEG C, then reaction mixture is pumped in pressure filter, pass into pressurized gas, press filtration under the pressure effect of pressurized gas (2-4 standard atmospheric pressure), makes reaction mixture realize solid-liquid separation, obtains filter cake and filtrate respectively;
The filter cake obtained puts into that prefabricated circular die is shaping, and filter cake is evenly distributed, and consistency of thickness (about 1-1.5cm), carries out centrifuge dehydration on this basis, centrifugal rotational speed 4500 turns/min, and after dehydration, effective constituent Content of Allantoin can reach 96%; Washing 1h is carried out to the wallantoin obtained after centrifugal, first uses 45 DEG C of hot wash 40min during washing, and then use tap water.
The filtrate that above-mentioned press filtration is separated contains excessive urea and hydrogen peroxide catalyzed dose, and this filtrate is dry via efficient centrifugal spraying machine, and drying temperature is 300 DEG C, and after dry, urea can be reduced into solid again, and as raw materials for production reuse, peroxide decomposition becomes gas.
Above content is only citing made for the present invention and explanation; affiliated those skilled in the art make various amendment to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
Claims (5)
1. a wallantoin production technique, this technique comprises: the reaction that feeds intake, press filtration and centrifuge washing step, it is characterized in that: in reactor, first add aqueous glyoxylic acid, urea and hydrogen peroxide catalyzed dose, stirring heating, after thing to be mixed reacts for some time, again in reactor, add a certain amount of urea, heat up to stir and continue reaction;
After having reacted, reaction mixture is cooled, then reaction mixture is pumped in pressure filter, pass into pressurized gas, make reaction mixture realize solid-liquid separation, obtain filter cake and filtrate respectively;
Above-mentioned filter cake is put into pre-formed, carries out centrifuge dehydration on this basis, and after dehydration, wallantoin washs, and first uses hot wash, and then with tap water; Above-mentioned filtrate is dry via efficient centrifugal spraying machine, and after dry, urea can be reduced into solid again.
2. a kind of wallantoin production technique according to claim 1, is characterized in that: by weight, and mass concentration is aqueous glyoxylic acid 1-1.5 part of 53-66%, urea 5-7 part, hydrogen peroxide catalyzed dose of 0.1-0.15 part.
3. a kind of wallantoin production technique according to claim 1, it is characterized in that: described stirring heating temperature is 85-90 DEG C, the reaction times is 3h, is again warming up to 95 DEG C, continues reaction 5h.
4. a kind of wallantoin production technique according to claim 1, it is characterized in that: after having reacted, reaction mixture is cooled to 30 DEG C, again reaction mixture is pumped in pressure filter, pass into pressurized gas, press filtration under 2-4 standard atmospheric pressure effect, makes reaction mixture realize solid-liquid separation.
5. a kind of wallantoin production technique according to claim 1, is characterized in that: described centrifugal rotational speed 3500 turns/min, and after dehydration, effective constituent Content of Allantoin can reach 95%; Washing 1h is carried out to the wallantoin obtained after centrifugal, first uses 30 DEG C of hot wash 20min during washing, and then use tap water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610145032.XA CN105541726A (en) | 2016-03-14 | 2016-03-14 | Allantoin production technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610145032.XA CN105541726A (en) | 2016-03-14 | 2016-03-14 | Allantoin production technology |
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| CN105541726A true CN105541726A (en) | 2016-05-04 |
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| CN201610145032.XA Pending CN105541726A (en) | 2016-03-14 | 2016-03-14 | Allantoin production technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083725A (en) * | 2016-06-12 | 2016-11-09 | 北京梅尔森医药技术开发有限公司 | A kind of preparation method of high-purity allantoin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103145621A (en) * | 2013-03-01 | 2013-06-12 | 凤台县精华助剂有限公司 | Allantoin preparation method |
-
2016
- 2016-03-14 CN CN201610145032.XA patent/CN105541726A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103145621A (en) * | 2013-03-01 | 2013-06-12 | 凤台县精华助剂有限公司 | Allantoin preparation method |
Non-Patent Citations (3)
| Title |
|---|
| 刘亚强等: "尿囊素的化学合成", 《宝鸡文理学院学报(自然科学版)》 * |
| 胡卫东: "尿素深加工技术两则", 《氮肥设计》 * |
| 胡震等: "乙二醛氧化-尿素缩合法合成尿囊素", 《四川化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083725A (en) * | 2016-06-12 | 2016-11-09 | 北京梅尔森医药技术开发有限公司 | A kind of preparation method of high-purity allantoin |
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Application publication date: 20160504 |