CN100422162C - Method for producing saccharin sodium - Google Patents
Method for producing saccharin sodium Download PDFInfo
- Publication number
- CN100422162C CN100422162C CNB2005100132266A CN200510013226A CN100422162C CN 100422162 C CN100422162 C CN 100422162C CN B2005100132266 A CNB2005100132266 A CN B2005100132266A CN 200510013226 A CN200510013226 A CN 200510013226A CN 100422162 C CN100422162 C CN 100422162C
- Authority
- CN
- China
- Prior art keywords
- water
- solution
- stirring
- acid
- ammonification
- 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.)
- Active
Links
Abstract
The present invention relates to a method for producing saccharin sodium, which comprises the steps of acyl ammonification, hofmann degradation esterification, diazotization, displacement, chlorination, ammonification, acid precipitation, alkalization reaction and decolorization reaction, and a finished product is obtained by filtration, concentration, crystallization and drying. The present invention is characterized in that the acid precipitation step and the alkalization reaction step mainly comprise: 15 to 30% of sulphuric acid is added to precipitate insoluble substances; toluene is added to ball up the insoluble substances; water is used for washing till acid water is clarified; edible sodium carbonate solution with the concentration of 10 to 30% is prepared and is added into insoluble rubber particles after the acid water is pumped; at the same time, the temperature is raised to 45 to 55 DEG C, and the pH value is from 2.8 to 3.8; stirring is carried out for 5 to 10 minutes; the solution is uniform and transparent solution, the stirring is stopped for still standing rest and delamination, and benzosulfimide natrium solution with the concentration of 20 to 25% is obtained. In the acid precipitation and alkalization reaction processes, liquid reacts. Because the temperature is low and the toluene is not easy to volatilize, air pollution is reduced, and the working environment of operators is improved. The method has the advantages of simple operation and effectively decreased labor intensity and production cost.
Description
Technical field
The present invention relates to a kind of foodstuff additive production method, particularly a kind of method for producing saccharin sodium.
Background technology
At present, soluble saccharin is as foodstuff additive, and range of application is very extensive.Its production method mainly comprises amidated, Hofmann degradation fatization, diazotization, displacement, chlorination, ammonification, acid out, alkalization and decoloring reaction step, more after filtration, concentrate, crystallization, drying obtain finished product.The wherein existing acid out that generally adopts, alkalization production method are to separate out insolublely with 31% hydrochloric acid, utilize in the solid sodium bicarbonate and insoluble micelle.This method labour intensity is big, needs at a large amount of raw materials that drop into 25 kilograms every bag of two meters eminences; While cost height, the existing market price of 31% hydrochloric acid is 550 yuan/ton, add particularly that solid sodium bicarbonate local heating is fast, temperature is high, speed of response is fast, reaction is violent, cause the rapid evaporative emission air of toxic substance toluene, be difficult to guarantee operator's good working environment, the pH value is difficult to measure control simultaneously, influences the preparation quality of soluble saccharin intermediate product.
Summary of the invention
The objective of the invention is to improve the various drawbacks that acid out in the above-mentioned method for producing saccharin sodium, quaternization process exist, a kind of simple to operate, method for producing saccharin sodium of reducing labour intensity, reducing atmospheric pollution, improve operating environment and reduce cost is provided.
The technical solution adopted in the present invention is for achieving the above object: a kind of method for producing saccharin sodium, comprise amidated, Hofmann degradation fatization, diazotization, displacement, chlorination, ammonification, acid out, alkalization and decoloring reaction step, concentrate again after filtration,, crystallization, drying obtain finished product, it is characterized in that wherein acid out, quaternization step are as follows:
(1) will stir in the ammonification liquid that make behind the aminating reaction and toluene wash water suction acid out, the quaternization still;
(2) adding water adjustment ammonification liquid and toluene wash water strength of solution is 1.05～1.06kg/m
3, it is long-pending to measure ammonification liquid, and ammonification liquid is 1500～1700 parts in proportion, adds toluene and continues for 375～425 parts to stir, and temperature is 18～20 ℃;
(3) adding 375～425 parts of concentration in stirring is 15%～30% sulfuric acid, and the time is 10～15 minutes, and temperature is 15～30 ℃, and measuring pH value is between 1～4, fully separating out insoluble micelle under the stirring, is the acid out terminal point with the sour water clarification;
(4) the sour water siphon is gone into reactor bottom subsider and discharge, keep 15～25 ℃ of temperature, stirred 10～20 minutes, emptying sour water in continuing stirring;
(5) the insoluble micelle of water repetitive scrubbing is till measure chloride content in the wash water≤0.08%;
(6) make pickling cover water with reclaiming in the last wash water suction disome water measuring tank;
(7) with 611～1100 parts of concentration be 10～30% edible sodium carbonate solution, add in the insoluble micelle that exhausts behind the sour water that the capping still stirs at interval, continues to start stirring after the decompression;
(8) simultaneously reactor is warming up to 45～55 ℃, evenly stirs to make the dissolving that all neutralizes of insoluble micelle and edible sodium carbonate solution, measures adjustment pH value of solution value and reaches 2.8～3.8;
(9) stirred 5～10 minutes, solution is homogeneous transparent solution, stops to stir standing demix, obtains 20～25% saccharin sodium solutions;
(10) carry out decoloring reaction routinely, more after filtration, concentrate, crystallization, drying obtain finished product.
The invention has the beneficial effects as follows: the sulfuric acid with concentration 15%～30% in acid out, the quaternization replaces 31% hydrochloric acid, with the existing market calculation of price: concentration is that 92% sulfuric acid is 650 yuan/ton, after being diluted to 15%～30%, 56～110 yuan of the every batch of consumption escapable costs significantly reduce the cost that raw material drops into.Raw material is directly squeezed into from Polycondensation Reactor and Esterification Reactor in the preparation, not be used in eminence and feeds intake, and is simple to operate, reduces labour intensity.This acid out, quaternization process are liquid reactions, and temperature of reaction is lower, and toluene is not volatile, and the atmospheric pollution that causes thereby avoid solid material to feed intake time reaction is violent effectively improves operator's Working environment; Simultaneously reaction process is steady, high quality and low cost, boosts productivity.
Embodiment
Below in conjunction with preferred embodiment, to details are as follows according to embodiment provided by the invention:
Embodiment 1:
A kind of method for producing saccharin sodium comprises amidated, Hofmann degradation fatization, diazotization, displacement, chlorination, ammonification, acid out, alkalization and decoloring reaction step, more after filtration, concentrate, crystallization, drying obtain finished product.This method for producing saccharin sodium mainly is to have improved acid out, quaternization preparation process, and aminating reaction obtains the main ingredient of intermediate ammonification liquid as acid out, quaternization;
The aminating reaction formula is:
Acid out, quaternization step are as follows:
(1) will stir in the ammonification liquid that make behind the aminating reaction and toluene wash water suction acid out, the quaternization still;
(2) adding water adjustment ammonification liquid and toluene wash water strength of solution is 1.05～1.06kg/m
3, it is long-pending to measure ammonification liquid, and ammonification liquid is 1600L in proportion, adds toluene 400L and continues to stir, and temperature is 18 ℃～20 ℃;
(3) adding 400L concentration in stirring is 22% sulfuric acid, and the time is 10～15 minutes, and temperature is 15～30 ℃, and measuring pH is between 1～4, separates out insoluble micelle under fully stirring, and observes insoluble micelle surface, with smooth, be advisable like red bean grain size; With the sour water clarification is the acid out terminal point;
The acid precipitation reaction formula is:
(4) the sour water siphon is gone into reactor bottom subsider and discharge, keep temperature to stir 10～20 minutes emptying sour water in continuing stirring for 15～25 ℃;
(5) wash insoluble micelle 4 times with water, each wash water is 500～800 kilograms, stirs while discharging water the water exhaustion, and repetitive scrubbing is till measure chloride content in the wash water≤0.08%;
(6) make pickling cover water with reclaiming in the last wash water suction disome water measuring tank;
(7) with 860L concentration be 20% edible sodium carbonate solution, add in the insoluble micelle that exhausts behind the sour water that the capping still stirs at interval, continues to start stirring after the decompression; The Yin Ben reaction has great amount of carbon dioxide to produce, for preventing just can normally to start stirring after dashing material should make pressure all disappear;
(8) simultaneously reactor is warming up to 50 ℃, evenly stirs to make the dissolving that all neutralizes of insoluble micelle and edible sodium carbonate solution be uniform solution, measures to adjust the pH value of solution value and reach 2.8～3.8;
The quaternization formula is:
(9) stirred 5～10 minutes, solution is homogeneous transparent solution, stops to stir to leave standstill its layering, lower floor are obtained in 20～25% saccharin sodium solution suction bleachers;
(10) carry out decoloring reaction routinely, more after filtration, concentrate, crystallization, drying obtain finished product.
Embodiment 2:
Acid out, quaternization step are as follows:
(1) will stir in the ammonification liquid that make behind the aminating reaction and toluene wash water suction acid out, the quaternization still;
(2) adding water adjustment ammonification liquid and toluene wash water strength of solution is 1.05～1.06kg/m
3, it is long-pending to measure ammonification liquid, and ammonification liquid is 1500L in proportion, adds toluene 375L and continues to stir, and temperature is 18 ℃～20 ℃;
(3) adding 375L concentration in stirring is 15% sulfuric acid, and the time is 10～15 minutes, and temperature is below 15～30 ℃, measuring pH is between 1～4, under fully stirring, separate out insoluble micelle, observe insoluble micelle surface, with smooth, be advisable like red bean grain size; With the sour water clarification is the acid out terminal point;
(4) the sour water siphon is gone into reactor bottom subsider and discharge, keep 15～25 ℃ of temperature, stirred 10～20 minutes, in continuing stirring, discharge sour water, and sour water is all pumped with vacuum;
(5) wash insoluble micelle 3 times with water, each wash water is 500～800 kilograms, stirs while discharging water the water exhaustion, and repetitive scrubbing is till measure chloride content in the wash water≤0.08%;
(6) make pickling cover water with reclaiming in the last wash water suction disome water measuring tank;
(7) with 611L concentration be 10% edible sodium carbonate solution, add in the insoluble micelle that exhausts behind the sour water that the capping still stirs at interval, continues to start stirring after the decompression; The Yin Ben reaction has great amount of carbon dioxide to produce, for preventing just can normally to start stirring after dashing material should make pressure all disappear;
(8) simultaneously reactor is warming up to 45 ℃, evenly stirs to make the dissolving that all neutralizes of insoluble micelle and edible sodium carbonate solution be uniform solution, measures to adjust the pH value of solution value and reach 2.8～3.8;
(9) stirred 5～10 minutes, solution is homogeneous transparent solution, stops to stir to leave standstill its layering, lower floor are obtained in 20～25% saccharin sodium solution suction bleachers;
(10) carry out decoloring reaction routinely, more after filtration, concentrate, crystallization, drying obtain finished product.
Other is with embodiment 1.
Embodiment 3:
Acid out, quaternization step are as follows:
(1) will stir in the ammonification liquid that make behind the aminating reaction and toluene wash water suction acid out, the quaternization still;
(2) adding water adjustment ammonification liquid and toluene wash water strength of solution is 1.05～1.06kg/m
3, it is long-pending to measure ammonification liquid, and ammonification liquid is 1700L in proportion, adds toluene 425L and continues to stir, and temperature is 18 ℃～20 ℃;
(3) adding 425L concentration in stirring is 30% sulfuric acid, and the time is 10～15 minutes, and temperature is at 15～30 ℃, and measuring pH is between 1～4, separates out insoluble micelle under fully stirring, and observes insoluble micelle surface, with smooth, be advisable like red bean grain size; With the sour water clarification is the acid out terminal point;
(4) the sour water siphon is gone into reactor bottom subsider and discharge, keep 15～25 ℃ of temperature, stirred 10～20 minutes, in continuing stirring, discharge sour water, and sour water is all pumped with vacuum;
(5) wash insoluble micelle 3～5 times with water, each wash water is 500～800 kilograms, stirs while discharging water the water exhaustion, and repetitive scrubbing is till measure chloride content in the wash water≤0.08%;
(6) make pickling cover water with reclaiming in the last wash water suction disome water measuring tank;
(7) with 1100L concentration be 30% edible sodium carbonate solution, add in the insoluble micelle that exhausts behind the sour water that the capping still stirs at interval, continues to start stirring after the decompression; The Yin Ben reaction has great amount of carbon dioxide to produce, for preventing just can normally to start stirring after dashing material should make pressure all disappear;
(8) simultaneously reactor is warming up to 55 ℃, evenly stirs to make the dissolving that all neutralizes of insoluble micelle and edible sodium carbonate solution be uniform solution, measures to adjust the pH value of solution value and reach 2.8～3.8;
(9) stirred 5～10 minutes, solution is homogeneous transparent solution, stops to stir to leave standstill its layering, lower floor are obtained in 20～25% saccharin sodium solution suction bleachers;
(10) carry out decoloring reaction routinely, more after filtration, concentrate, crystallization, drying obtain finished product.
Other is with embodiment 1.
Claims (1)
1. method for producing saccharin sodium, comprise amidated, Hofmann degradation fatization, diazotization, displacement, chlorination, ammonification, acid out, alkalization and decoloring reaction step, concentrate again after filtration,, crystallization, drying obtain finished product, it is characterized in that wherein acid out, quaternization step are as follows:
(1) will stir in the ammonification liquid that make behind the aminating reaction and toluene wash water suction acid out, the quaternization still;
(2) adding water adjustment ammonification liquid and toluene wash water strength of solution is 1.05～1.06kg/m
3, it is long-pending to measure ammonification liquid, and ammonification liquid is 1500～1700 parts in proportion, adds toluene and continues for 375～425 parts to stir, and temperature is 18～20 ℃;
(3) adding 375～425 parts of concentration in stirring is 15%～30% sulfuric acid, and the time is 10～15 minutes, and temperature is 15～30 ℃, and measuring pH value is between 1～4, fully separating out insoluble micelle under the stirring, is the acid out terminal point with the sour water clarification;
(4) the sour water siphon is gone into reactor bottom subsider and discharge, keep 15～25 ℃ of temperature, stirred 10～20 minutes, emptying sour water in continuing stirring;
(5) the insoluble micelle of water repetitive scrubbing is till measure chloride content in the wash water≤0.08%;
(6) make pickling cover water with reclaiming in the last wash water suction disome water measuring tank;
(7) with 611～1100 parts of concentration be 10～30% edible sodium carbonate solution, add in the insoluble micelle that exhausts behind the sour water that the capping still stirs at interval, continues to start stirring after the decompression;
(8) simultaneously reactor is warming up to 45～55 ℃, evenly stirs to make the dissolving that all neutralizes of insoluble micelle and edible sodium carbonate solution, measures adjustment pH value of solution value and reaches 2.8～3.8;
(9) stirred 5～10 minutes, solution is homogeneous transparent solution, stops to stir standing demix, obtains 20～25% saccharin sodium solutions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100132266A CN100422162C (en) | 2005-03-22 | 2005-03-22 | Method for producing saccharin sodium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100132266A CN100422162C (en) | 2005-03-22 | 2005-03-22 | Method for producing saccharin sodium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1663429A CN1663429A (en) | 2005-09-07 |
| CN100422162C true CN100422162C (en) | 2008-10-01 |
Family
ID=35034878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100132266A Active CN100422162C (en) | 2005-03-22 | 2005-03-22 | Method for producing saccharin sodium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100422162C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439257C (en) * | 2006-07-10 | 2008-12-03 | 天津北方食品有限公司 | Method for treating acid-extracted waste liquid used for production of saccharin sodium |
| CN101786998B (en) * | 2010-04-08 | 2011-07-20 | 天津市鑫卫化工有限责任公司 | Preparation method of high-purity o-sulfonylbenzoylimine |
| CN103183622B (en) * | 2011-12-29 | 2014-06-18 | 河南大学 | 2-ammonium sulphonate methyl benzoate and synthetic process thereof |
| CN103709118B (en) * | 2013-12-19 | 2015-10-07 | 中国平煤神马集团开封兴化精细化工有限公司 | A kind of production method of soluble saccharin |
| CN104402760B (en) * | 2014-09-28 | 2018-05-25 | 中国平煤神马集团开封兴化精细化工有限公司 | Diazo-reaction continuous production method in a kind of saccharin production process |
| CN105085333B (en) * | 2015-08-07 | 2017-07-04 | 新乡市辉普化工科技有限公司 | The preparation method of first sulfanilamide (SN) |
| AU2016380889B2 (en) * | 2016-01-01 | 2021-02-18 | Adama Agan Ltd. | Process for preparing 1.1.3-Trioxo-1.2-benzothiazole-6-carboxamide |
| CN108101862A (en) * | 2018-01-10 | 2018-06-01 | 江西富味特生物技术有限公司 | A kind of preparation method of saccharin sodium |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1478773A (en) * | 2003-07-03 | 2004-03-03 | 齐化多 | Production technology of scaccharin sodium salt |
-
2005
- 2005-03-22 CN CNB2005100132266A patent/CN100422162C/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1478773A (en) * | 2003-07-03 | 2004-03-03 | 齐化多 | Production technology of scaccharin sodium salt |
Non-Patent Citations (2)
| Title |
|---|
| 糖精钠的清洁生产. 施剑波.精细与专用化学品，第2003卷第11期. 2003 |
| 糖精钠的清洁生产. 施剑波.精细与专用化学品，第2003卷第11期. 2003 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1663429A (en) | 2005-09-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100422162C (en) | Method for producing saccharin sodium | |
| CN206604491U (en) | A kind of automatically cleaning stirred autoclave | |
| CN109603609A (en) | A kind of fertilizer production quick agitator | |
| CN105712887B (en) | A kind of production method of long-chain nylon salt | |
| CN101671374B (en) | New technique for extracting D-glucosamine hydrochloride | |
| CN112158865A (en) | Method for recycling lithium element in lithium precipitation mother liquor | |
| CN110330439A (en) | A kind of zinc-glycine complex and preparation method thereof not introducing foreign ion | |
| CN1615722A (en) | Method for preparing soybean separate protein by ultra-filter film separation technology | |
| CN101367554B (en) | Method for preparing potassium manganate solution | |
| CN208213157U (en) | A kind of water treatment agent reaction kettle with high-efficiency stirring | |
| CN110818770A (en) | Method for preparing diosgenin by ternary biphase aluminum chloride hydrolysis | |
| CN108530291A (en) | A kind of continuous acidolysis method of calcium hydrogen citrate | |
| CN104744365A (en) | Method for directly preparing light-emitting material 8-hydroxyquinoline copper | |
| CN1046293C (en) | Modified corn starch dyeing paste and its preparation | |
| CN105712888B (en) | A kind of preparation method of long-chain nylon salt | |
| CN113955776A (en) | Preparation method of lithium carbonate | |
| CN102951626A (en) | Method for preparing high-purity stannous pyrophosphate | |
| CN208856921U (en) | A kind of production line of nickelous carbonate | |
| CN206262393U (en) | One kind stirring paste producing device | |
| CN106809811B (en) | A method of sodium pyrophosphate is prepared using crude product sodium pyrophosphate | |
| CN109225148A (en) | It is a kind of improve washing efficiency filter aid and its application | |
| CN102921365A (en) | Enamel flat-bottom concentration reaction vessel | |
| CN114380315B (en) | Purification method and production equipment of medicinal calcium carbonate | |
| CN218250195U (en) | 2,4-dinitrochlorobenzene preparation neutralization washing machine | |
| CN109053629A (en) | Tubular reactor sodium hypochlorite is the accelerator DZ and method of oxidant production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |