CN1478773A - Production technology of scaccharin sodium salt - Google Patents
Production technology of scaccharin sodium salt Download PDFInfo
- Publication number
- CN1478773A CN1478773A CNA031262392A CN03126239A CN1478773A CN 1478773 A CN1478773 A CN 1478773A CN A031262392 A CNA031262392 A CN A031262392A CN 03126239 A CN03126239 A CN 03126239A CN 1478773 A CN1478773 A CN 1478773A
- Authority
- CN
- China
- Prior art keywords
- soluble saccharin
- asccharin
- water
- saccharin
- mother liquor
- 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
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 159000000000 sodium salts Chemical class 0.000 title description 2
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims abstract description 52
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000013078 crystal Substances 0.000 claims description 17
- 239000012452 mother liquor Substances 0.000 claims description 14
- 235000017550 sodium carbonate Nutrition 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 150000008064 anhydrides Chemical class 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001953 recrystallisation Methods 0.000 claims description 3
- 239000006260 foam Substances 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 3
- 229940081974 saccharin Drugs 0.000 abstract description 2
- 235000019204 saccharin Nutrition 0.000 abstract description 2
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 abstract description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 24
- 239000002994 raw material Substances 0.000 description 21
- 235000017557 sodium bicarbonate Nutrition 0.000 description 12
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- 239000011734 sodium Substances 0.000 description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 5
- 239000011541 reaction mixture Substances 0.000 description 5
- NWYRNCMKWHKPAI-UHFFFAOYSA-N C(=O)=O.[Na] Chemical compound C(=O)=O.[Na] NWYRNCMKWHKPAI-UHFFFAOYSA-N 0.000 description 3
- 230000000711 cancerogenic effect Effects 0.000 description 3
- 231100000315 carcinogenic Toxicity 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 230000001143 conditioned effect Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 235000003599 food sweetener Nutrition 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229940085605 saccharin sodium Drugs 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000003765 sweetening agent Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 208000007097 Urinary Bladder Neoplasms Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005183 environmental health Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Saccharide Compounds (AREA)
Abstract
A process for preparing sodium saccharin includes such steps as reaction of sodium carbonate on saccharin, decoloring, filtering, and crystallizing. Its advantages are less increasement in volume of mother liquid, less generation of CO2 and foam, and low cost.
Description
Technical field
The present invention relates to a kind of soluble saccharin production technique, is the production technique of raw material production soluble saccharin with yellow soda ash and asccharin particularly.
Background technology
The chemical name of asccharin is a saccharin, and molecular formula is: C
7H
5O
3NS, structural formula is:
Melting range is 228-230 ℃, is colourless crystallization, or white powder, and its sugariness is about 500 times of sucrose, and is water insoluble, claims saccharin insoluble or saccharinic acid again.And soluble saccharin is the sodium salt of asccharin, and is soluble in water, claims soluble saccharin again, is colourless to white rhombic system plate crystal, and odorless or little aromatic odour arranged can not be by metabolism in human body, and calorific value is zero.Soluble saccharin can be used as sweetening agent.
Edible safety problem about asccharin worldwide had dispute, was once suspecting once that asccharin might make the people carcinogenic.Point out in the carcinogenic problem report and issue in American National Environmental Health Science Institute, test shows, asccharin causes the situation of mouse tumor of bladder and is not suitable on one's body the mankind, and in Mays 15 in 2000 Japan-US state government announce asccharin is deleted from carcinogenic material list, (see the report of " United States Government announces that " asccharin be harmful to health opinion " lacks scientific basis " of the publication of on June 23rd, 2000 " Chinese chemical industry newspaper " and on July 26th, 2000 " China Intellectual Property News ".) and comprised that from asccharin in 2002 more than 100 countries and regions approval of the U.S., China use as sweetening agent.
Usually, producing soluble saccharin and be with food grade sodium bicarbonate and asccharin is raw material, by chemical reaction, and decolouring, filtration, crystallization, spissated method, and produce the saccharin sodium powder or require the soluble saccharin crystal of size (certain order number).Its chemical equation is:
Sodium bicarbonate be by food-grade anhydrous yellow soda ash in solution with carbon dioxide reaction or by the crystals of sodium carbonate that contains crystal water and carbon dioxide reaction and make.And food grade yellow soda ash is to adopt soda and sociation center to claim that Hou's process for soda production is that raw material is produced anhydrous sodium carbonate and ammonium chloride respectively with ammonia, salt, carbonic acid gas and water.Owing in existing soluble saccharin production technique, be to use sodium bicarbonate and asccharin to make raw material, thereby in the process of chemical reaction, can produce a large amount of CO
2Gas, and, be easy to generate the still phenomenon of overflowing because of the conference of reaction solution viscosity forms a large amount of foams, material is overflowed outside the still, this not only can cause wastage of material, but also can make troubles to operation.And, when after crystallization and recrystallization operation, separating crystal grain and mother liquor, the mother liquor that needs water flushing grain surface, cause soluble saccharin mother liquor volume growth speed very fast, wayward, reduce in order to make soluble saccharin mother liquor volume, just must concentrate, will increase like this and produce man-hour, production cost is improved.
Summary of the invention
The object of the present invention is to provide a kind of soluble saccharin production technique, it is with Na
2CO
3With asccharin be that raw material is produced, can overcome the deficiency of prior art, can control the growth of soluble saccharin mother liquor volume in the production process effectively; And can reduce CO in the reaction process effectively
2Foamy produces, and is difficult for the still that overflows; Can reduce production costs effectively simultaneously.
The present invention is to be raw material with yellow soda ash and asccharin, produces soluble saccharin by chemical reaction, and its chemical equation is:
And adopt following production craft step:
In reactor, add water or soluble saccharin mother liquor 2-5 part, add yellow soda ash again (with Na
2CO
3Pure meter) 1 part and asccharin are (with C
7H
5O
3The pure meter of SN) 3.4 parts, stir, heat, carry out chemical reaction, CO is arranged in the reaction process
2Gas generates.Treat that temperature rises to about 70 ℃, yellow soda ash has dissolved, and reactant is by thick when thinning, adjust PH to 7.0, concentration transfers to 31-34Be, carries out heat filtering under the state of temperature between 60-100 ℃, then, crystallization or recrystallization, separate crystal grain and mother liquor, remove the grain surface attached water, sub-sieve, make finished product, this finished product is the soluble saccharin dihydrate.
Described yellow soda ash comprises anhydride Na
2CO
3One water thing Na
2CO
3H
2O; Seven water thing Na
2CO
37H
2O; Ten water thing Na
2CO
310H
2O.Preferred food product level anhydride Na of the present invention
2CO
3
Because the present invention is raw material with yellow soda ash and asccharin, by chemical reaction, decolorization filtering, crystallization and produce the soluble saccharin crystal that saccharin sodium powder or institute require big or small (necessarily order number).Compare as raw material with using sodium bicarbonate, when the soluble saccharin of production equivalent, can reduce the CO of half
2The generation of gas, thereby the CO that produces
2Foam is also few.From chemical equation (I) as can be seen, use sodium bicarbonate whenever to make 1 soluble saccharin molecule, just have 1 CO as raw material
2Molecule generates; And from chemical equation (II) as can be seen, be 2 soluble saccharin molecules of the every production of raw material with yellow soda ash, just have 1 CO
2Molecule generates.Obviously the present invention is that the raw material ratio prior art is the CO that raw material produces with the sodium bicarbonate with yellow soda ash
2Gas is wanted much less, the CO that produces in the reaction process
2The gas foam is much less also, like this, not only can prevent flash effectively, reduces the waste of raw material, but also handled easily.
Moreover, from chemical equation (II) as can be seen, each Carbon Dioxide sodium molecule can from chemical equation (I) as can be seen, each sodium bicarbonate molecule can generate the soluble saccharin dihydrate with the asccharin molecular reaction together with 1 water molecules with asccharin molecular reaction generation soluble saccharin dihydrate together with 3 water moleculess.Therefore, the present invention uses anhydrous sodium carbonate to make raw material ratio prior art use sodium bicarbonate and makes raw material, can more help controlling the growth of soluble saccharin mother liquor volume in the production process, thereby can solve the fast problem of soluble saccharin mother liquor volume growth in the soluble saccharin production technique better, therefore can save the soluble saccharin mother liquor is carried out spissated step, simplify processing step, shorten man-hour.
In addition, from chemical equation (I) as can be seen, 1 soluble saccharin molecule of every production will have 1 sodium bicarbonate molecule to participate in reaction, and from chemical equation (II) as can be seen, 2 soluble saccharin molecules of every production just need 1 Carbon Dioxide sodium molecule to participate in reaction.The required weight of anhydrous sodium carbonate of using of 1 ton of soluble saccharin of every production is 220kg, and the required weight with sodium bicarbonate of 1 ton of soluble saccharin of every production is 348kg in the existing technology, like this, the weight of the used Carbon Dioxide sodium raw materials of the present invention lacks 36.7% than the weight of used sodium bicarbonate raw material in the prior art.And with regard to the market value of above-mentioned two kinds of raw materials, be more or less the same, at present, the price of anhydrous sodium carbonate is 1010-1390 unit/ton, and the price of sodium bicarbonate is 1400 yuan/ton (seeing on June 19th, 2003 " Chinese chemical industry newspaper " the 3rd edition).This shows, the present invention uses anhydrous sodium carbonate to make raw material and prior art to use sodium bicarbonate to compare as raw material, and it is few to have a consumption, the advantage that can reduce production costs effectively, at current price conservative calculating produced soluble saccharin per ton and can be reduced cost more than 200 yuan.
Description of drawings
Accompanying drawing is the process flow sheet of raw material production soluble saccharin with yellow soda ash and asccharin for the present invention.
Embodiment
Further describe embodiment below in conjunction with embodiment.
Embodiment 1:
Add 100ml distilled water in the 2000ml beaker, intersect and add anhydrous sodium carbonate 40g and 90% the asccharin 150g of giving money as a gift, stir, heating keeps reaction mixture to be alkalescence, has a large amount of foams to generate in the reaction mixture, and this foam gas is CO
2After the thinning clarification of reaction mixture, P
HValue is still greater than 7.0.Show that asccharin has reacted, continue to add above-mentioned an amount of asccharin, stir, be adjusted to reaction solution P
HValue is 7.0.In the time of 80 ℃, it is an amount of to add water, and conditioned reaction liquid concentration is 33Be.Add activated carbon 2g, continue to stir 20 minutes, heat tracing carries out heat filtering for about 90 ℃.Filtrate moved into carry out spontaneous nucleation in the glass crystallization kettle.Soluble saccharin solution is under 7.0 the neutral state at pH value, when temperature is reduced to 55 ℃, cooling rate is slowed down to 8-10 minute and is fallen 1 ℃, make soluble saccharin crystal grain separate out and grow, last till always and when temperature drops to 25 ℃ crystal is separated with liquid glucose, after washing with water, through centrifuge dripping, airing surface attachment moisture gets soluble saccharin crystal 75g again.Chemically examine according to GB4578-84 soluble saccharin national standard: content is 99.1%, and heavy metal (in Pb) is less than 5ppm, moisture: 14.2%, and quality meets GB4578-84 soluble saccharin national standard.
Embodiment 2:
In the 2000ml beaker, add 200ml soluble saccharin mother liquor, intersect again and add anhydrous sodium carbonate 50g and 89% the asccharin 190g of giving money as a gift, stir, heating, keep reaction mixture to be alkalescence, reaction mixture when thinning, adds an amount of asccharin mother liquid of sodium by thick, and preliminary examination concentration is 35Be.Treat that temperature is raised to 80 ℃, after asccharin has dissolved, add above-mentioned an amount of asccharin, stir, be adjusted to reaction solution P
HValue is 7.0, adds an amount of asccharin mother liquid of sodium, and conditioned reaction liquid concentration is to 32.5Be.Add gac 3g, continue to stir 20 minutes, be incubated 90 ℃ and carry out heat filtering, filtrate is moved in the glass crystallization kettle.Soluble saccharin solution is at P
HValue is when being cooled to 54 ℃ under 7.0 the neutral state, adds 20g crosses through sub-sieve, complete, the evengranular soluble saccharin crystal seed of corner angle, to descend 1 ℃ speed cooling in 8-10 minute.When dropping to 47 ℃, crystal solution becomes mixes, and has a large amount of soluble saccharin crystallites to separate out.Heat temperature raising to 52 ℃, liquid glucose is clear by muddy change, little crystallite off-bottom, to fall 1 ℃ speed cooling in 8-10 minute, when being cooled to 42 ℃, reheat is risen again to 48 ℃, rises again so repeatedly 6 times again.When the crystal solution temperature is reduced to 27 ℃, separate crystal grain and mother liquor, bath washing crystal grain, centrifuge dripping again through airing grain surface attached water, gets soluble saccharin crystal 2 31g.Chemically examine according to GB4578-84 soluble saccharin national standard, content is 99.3%, and heavy metal (in Pb) is less than 5ppm, moisture: 14.1%, and quality meets GB4578-84 soluble saccharin national standard.
Claims (2)
1, a kind of soluble saccharin production technique, its feature comprises following processing step,
(1) in reactor, adds water or soluble saccharin mother liquor, add yellow soda ash and asccharin again, stir and heating, carry out chemical reaction;
(2) in 60-100 ℃ temperature range, carry out heat filtering;
(3) carry out crystallization or recrystallization;
(4) separate crystal grain and mother liquor, remove the grain surface attached water, make finished product, this finished product is the soluble saccharin dihydrate.
2, a kind of soluble saccharin production technique as claimed in claim 1 is characterized in that yellow soda ash comprises anhydride Na
2CO
3, a water thing Na
2CO
3H
2O, seven water thing Na
2CO
37H
2O, and ten water thing Na
2CO
310H
2O, preferred anhydride Na
2CO
3
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031262392A CN1478773A (en) | 2003-07-03 | 2003-07-03 | Production technology of scaccharin sodium salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031262392A CN1478773A (en) | 2003-07-03 | 2003-07-03 | Production technology of scaccharin sodium salt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1478773A true CN1478773A (en) | 2004-03-03 |
Family
ID=34153065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA031262392A Pending CN1478773A (en) | 2003-07-03 | 2003-07-03 | Production technology of scaccharin sodium salt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1478773A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100422162C (en) * | 2005-03-22 | 2008-10-01 | 天津北方食品有限公司 | Production method of sodium saccharin |
| CN110776476A (en) * | 2019-12-02 | 2020-02-11 | 北京海泰天正医药科技有限公司 | Medicinal o-benzoyl sulfonyl imide salt and preparation method thereof |
-
2003
- 2003-07-03 CN CNA031262392A patent/CN1478773A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100422162C (en) * | 2005-03-22 | 2008-10-01 | 天津北方食品有限公司 | Production method of sodium saccharin |
| CN110776476A (en) * | 2019-12-02 | 2020-02-11 | 北京海泰天正医药科技有限公司 | Medicinal o-benzoyl sulfonyl imide salt and preparation method thereof |
| CN110776476B (en) * | 2019-12-02 | 2021-06-08 | 北京海泰天正医药科技有限公司 | Medicinal o-benzoyl sulfonyl imide salt and preparation method thereof |
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|---|---|---|---|
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| PB01 | Publication | ||
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| RJ01 | Rejection of invention patent application after publication |