CN1080713C - Method for preparing gamma crystalline form sorbic alcohol - Google Patents
Method for preparing gamma crystalline form sorbic alcohol Download PDFInfo
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- CN1080713C CN1080713C CN98100433A CN98100433A CN1080713C CN 1080713 C CN1080713 C CN 1080713C CN 98100433 A CN98100433 A CN 98100433A CN 98100433 A CN98100433 A CN 98100433A CN 1080713 C CN1080713 C CN 1080713C
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- sorbyl alcohol
- crystal formation
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Abstract
The present invention relates to a method for preparing gamma crystalline form sorbic alcohol, which is characterized in that the sorbic alcohol of which the concentration is from 50 to 70% is concentrated to the sorbic alcohol of which the concentration is more than 90 %; the sorbic alcohol is in a molten state; then, the sorbic alcohol and crystalline seeds are mixed in a certain proportion; the temperature of the sorbic alcohol in the molten state is controlled from 90 to 94 DEGC; then, the sorbic alcohol containing a certain amount of gamma crystalline forms can be obtained by using the segment temperature control method. The method of the present invention saves alcohol, and thus, reduces investments on equipment, and lowers the production cost.
Description
The present invention relates to r crystal formation The Preparation of Crystal Sorbitol method.
R crystal formation sorbyl alcohol is mainly used in the sweeting agent and nice and cool agent, mouthfeel toughener, toughner, sanitas, tenderizer, the vehicle used of sugarfree foods.The preparation method of known r crystal formation sorbyl alcohol is the crystal seed that 70% sorbyl alcohol is added 30% (weight), add ethanol then, in crystallizer tank, utilize ethanol to make the sorbyl alcohol in the liquid be deposited on the crystal seed gradually to the avidity of water, and on crystal seed, grow, behind certain hour, take out xln, promptly obtain crystalline sorbitol by centrifugal drying, ethanol recycling use in the residue mother liquor, mother liquor also can continue to use (Process Techned Proc.1989.6 (Ind.cryst.87), 551-4 (Eng)).This technical process energy consumption is big, and alcohol consumption quantity and facility investment are big, complex process, thus make product cost very high.
The preparation method who the purpose of this invention is to provide the r crystal formation sorbyl alcohol that a kind of technology is simple, cost is low.
Main technical schemes of the present invention: the sorbyl alcohol with 50-70% concentration is concentrated into 98% above concentration earlier, add crystal seed again, temperature by control molten sorbyl alcohol makes its crystallization, and the crystalline sorbyl alcohol promptly obtains pulverous r crystal formation sorbyl alcohol through cooling off, pulverize, sieving.
Concrete preparation process of the present invention is followed successively by:
1, in vaporizer, under 922.254-1333.22 handkerchiefs, 100-110 ℃ condition, it is more than 98% that the sorbyl alcohol of 50-70% concentration is concentrated into concentration, and temperature is the sorbyl alcohol of 90-94 ℃ molten;
2, be that the sorbyl alcohol of 98% above molten becomes the magma mixture with crystal seed with 4-5: 1 mixed with (1) step concentration, temperature is controlled at 90-94 ℃;
3, with (2) but to put into the crystallizer tank employing temperature control method of the insulation can that places attemperation be the segmentation temperature that falls progressively to step magma mixture: reduced to 80-82 ℃ at 2-2.5 hours from 90-94 ℃ for first section, in 3-3.4 hours, reduce to 60-62 ℃ for second section, in 4-4.2 hours, reduce to 50-55 ℃, obtain containing the crystalline sorbitol of r crystal formation 70-85% for the 3rd section;
4, take out crystalline sorbitol and be cooled to room temperature, the r crystal formation sorbyl alcohol of pulverizing again, sieving and promptly obtain powder crystallization.This crystal formation sorbyl alcohol can be used as (2) step crystal seed.
Described crystal seed, market can have been bought, " the hard sorbyl alcohol " that the present invention uses Nanning chemical research institute to produce with the alcohol method, promptly r-crystal formation content is 60-85%, mean particle size is 60-80 purpose sorbyl alcohols.
Described insulation can, temperature can be regulated, and can place crystallizer tank in insulation can.
Major advantage of the present invention: the present invention is owing to adopt fusion temperature control method to obtain required r crystal formation sorbyl alcohol, thereby saved ethanol, reduces facility investment, and production cost only reaches 1/3rd of Ethanol Method.
Further specify characteristics of the present invention with embodiment below.
The method that following example r crystal formation content detection method employing " Shi Qingdong, " differential scanning amount method is measured r crystal formation content in the crystalline sorbitol ", in February, 1996 " provides.
Embodiment 1
This example is that the sorbyl alcohol of 70% concentration is concentrated into concentration under 1066.576 handkerchiefs, 100-110 ℃ be 98%, temperature is the sorbyl alcohol 40kg of 93 ℃ molten, being mixed into temperature with the 70 purpose crystal seeds of 10kg then is 92 ℃ magma mixture, this mixture is placed crystallizer tank in the insulation can, divide three sections slowly coolings: in 2 hours, reduce to 80 ℃ for first section from 92 ℃, in 3 hours, reduce to 60 ℃ for second section from 80 ℃, in 4 hours, reduce to 50 ℃ for the 3rd section from 60 ℃, obtain the 50kg crystalline sorbitol, its r crystal formation content is 78%.Used crystal seed is that r-crystal formation content is 68% sorbyl alcohol.
Embodiment 2
The experimentation of present embodiment, consumption, the temperature of crystal seed and sorbyl alcohol are identical with embodiment 1, temperature control: first section 2.5 hours, second section 3.4 hours, the 3rd section 4.2 hours, obtain r crystal formation content and be 84% sorbyl alcohol.
Embodiment 3
Present embodiment be the sorbyl alcohol temperature of molten be 98 ℃, other condition is with embodiment 1, r crystal formation content is 35% in the gained crystalline sorbitol, illustrates that the part crystal seed had dissolved when molten sorbyl alcohol temperature was too high.
Embodiment 4
Present embodiment be the sorbyl alcohol temperature of molten be 85 ℃, other condition is with embodiment 1, the brilliant content of r is 42% in the gained crystalline sorbitol, crystalline rate was also low when data declaration molten sorbyl alcohol temperature was low.
Embodiment 5
Present embodiment be the blending ratio of crystal seed and molten sorbyl alcohol be 1: 4, other condition is with embodiment 1, r crystal formation content is 73% in the gained crystalline sorbitol.
Claims (3)
1, a kind of method for preparing r crystal formation sorbyl alcohol is characterized in that preparation process is followed successively by:
(1) in vaporizer in 922.254-1333.22 handkerchief, 100-110 ℃, it is more than 98% that the sorbyl alcohol of 50-70% concentration is concentrated into concentration, temperature is the sorbyl alcohol of 90-94 ℃ molten;
(2) be that molten sorbyl alcohol and crystal seed more than 98% is mixed into the magma mixture with 4-5: 1 with concentration, the temperature of control mixture is 90-94 ℃;
(3) with (2) but to put into the crystallizer tank employing temperature control method of the insulation can that places attemperation be the segmentation temperature that falls progressively to step 90-94 ℃ of magma mixtures: reduced to 80-82 ℃ at 2-2.5 hours from 90-94 ℃ for first section, in 3-3.4 hours, reduce to 60-62 ℃ for second section, in 4-4.2 hours, reduce to 50-55 ℃, obtain containing the crystalline sorbitol of r crystal formation 70-85% for the 3rd section;
(4) take out crystalline sorbitol, be cooled to room temperature, the r crystal formation sorbyl alcohol of pulverizing again, sieving and promptly obtain powder crystallization.
2, in accordance with the method for claim 1, it is characterized in that r crystal formation content in the crystal seed is 60-85%, mean particle size 60-80 purpose sorbyl alcohols.
3, in accordance with the method for claim 1, it is characterized in that (4) step obtains r crystal formation sorbyl alcohol and can be used as (2) step crystal seed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98100433A CN1080713C (en) | 1998-02-19 | 1998-02-19 | Method for preparing gamma crystalline form sorbic alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98100433A CN1080713C (en) | 1998-02-19 | 1998-02-19 | Method for preparing gamma crystalline form sorbic alcohol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1188097A CN1188097A (en) | 1998-07-22 |
| CN1080713C true CN1080713C (en) | 2002-03-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98100433A Expired - Fee Related CN1080713C (en) | 1998-02-19 | 1998-02-19 | Method for preparing gamma crystalline form sorbic alcohol |
Country Status (1)
| Country | Link |
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| CN (1) | CN1080713C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172496B (en) * | 2012-11-22 | 2014-11-26 | 山东绿健生物技术有限公司 | Preparation method of gamma-crystalline sorbitol |
| CN104478662B (en) * | 2014-12-29 | 2015-12-02 | 临沂市鑫轮化工有限公司 | A kind of γ-crystal formation solid Sorbitol Powder continuous production method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030617A (en) * | 1987-06-29 | 1989-01-25 | 耐用电极株式会社 | Be used for electrolytic negative electrode and preparation method thereof |
| CN1035510A (en) * | 1988-02-20 | 1989-09-13 | 株式会社上野制药应用研究所 | The preparation method of solid sorbitol |
-
1998
- 1998-02-19 CN CN98100433A patent/CN1080713C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030617A (en) * | 1987-06-29 | 1989-01-25 | 耐用电极株式会社 | Be used for electrolytic negative electrode and preparation method thereof |
| CN1035510A (en) * | 1988-02-20 | 1989-09-13 | 株式会社上野制药应用研究所 | The preparation method of solid sorbitol |
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| Publication number | Publication date |
|---|---|
| CN1188097A (en) | 1998-07-22 |
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