CN109607480A - A kind of waste hydrochloric acid edulcoration purification process in Sucralose chlorination reaction - Google Patents
A kind of waste hydrochloric acid edulcoration purification process in Sucralose chlorination reaction Download PDFInfo
- Publication number
- CN109607480A CN109607480A CN201811504642.XA CN201811504642A CN109607480A CN 109607480 A CN109607480 A CN 109607480A CN 201811504642 A CN201811504642 A CN 201811504642A CN 109607480 A CN109607480 A CN 109607480A
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- CN
- China
- Prior art keywords
- hydrochloric acid
- waste hydrochloric
- waste
- enamel still
- sulfur dioxide
- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
- B01D53/501—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound
- B01D53/502—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound characterised by a specific solution or suspension
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/304—Alkali metal compounds of sodium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
- B01D2251/604—Hydroxides
Abstract
The present invention relates to the waste hydrochloric acid edulcoration purification process in a kind of Sucralose chlorination reaction, comprising the following steps: 1) waste hydrochloric acid removes insoluble impurities carbide, sulfide through filters pressing, then waste hydrochloric acid is pressed into closed enamel still；2) stirring is warming up to 45 DEG C -60 DEG C, and 30% hydrogen peroxide is added dropwise, and temperature is controlled at 50 ± 5 DEG C, until stopping reaction when bubble-free；3) gas phase generated in enamel still absorbs sulfur dioxide, HCl gas in gas phase by caustic wash tower lye；4) material in enamel still is cooled to 20 ± 5 DEG C, and concentration 30%, content of sulfur dioxide 0.01%, solution are obtained after filters pressing in flaxen hydrochloric acid.The present invention treated hydrochloric acid, purity is higher, and use scope is wider, than solid waste, the waste water that conventional method reduces HCl treatment；Treated hydrochloric acid, can produce chloroethanes.
Description
Technical field
The invention belongs to chemical production technical fields, are related to a kind of Sucralose chlorination generation waste hydrochloric acid edulcoration purification
Method.
Background technique
Sucralose (Sucralose or TGS CNS:19.016;INS:955), also known as Sucralose, sucrose essence or 4,
1,6 ,-three chloro- 4,1,6 ,-three deoxidation gala type sucrose, English name: Sucralose.Sucralose is to be with sucrose
Raw material is through prepared by chlorination.Thionyl chloride is main to generate hydrogen chloride and two as chlorinating agent during high-temp chlorination
Sulfur oxide tail gas, absorbs through tertiary effluent, the aqueous hydrochloric acid solution of formation.The a large amount of main sulfur-bearing series that its chlorination process generates
The hydrochloric acid of impurity, hydrochloric acid (Hydrochloric acid) molecular formula HCl, relative molecular mass 36.46.Hydrochloric acid is various concentration
Hydrochloride aqueous solution, be transparent and colorless or yellow, irritant smell and strong corrosive.Soluble easily in water, ethyl alcohol, ether and oil
Deng.Concentrated hydrochloric acid be the aqueous solution containing 38% hydrogen chloride, relative density 1.19, -112 DEG C of fusing point, -83.7 DEG C of boiling point.
Summary of the invention:
It is an object of the invention to provide a kind of methods for the waste hydrochloric acid edulcoration purification that Sucralose chlorination reaction generates, and reach drop
Impurity content in less salt aqueous acid, achievees the purpose that edulcoration purification.
The purpose of the present invention is what is be achieved by the following technical programs:
A kind of waste hydrochloric acid edulcoration purification process in Sucralose chlorination reaction, including Sucralose high-temperature chlorination step produce
Raw tail gas absorbs the waste hydrochloric acid for the concentration 30% to be formed with water, it is characterised in that the following steps are included:
1) waste hydrochloric acid removes insoluble impurities carbide, sulfide by plate and frame filter press, is then pressed into waste hydrochloric acid closed
Enamel still；
2) enamel still stirring to be opened, is warming up to 45 DEG C -60 DEG C, 30% hydrogen peroxide is added dropwise, temperature is controlled at 50 ± 5 DEG C, until
When bubble-free, stop reaction；
3) gas phase generated in enamel still absorbs sulfur dioxide, HCl gas in gas phase with lye by caustic wash tower；
4) for the feed liquid in enamel still through circulating water cooling to 20 ± 5 DEG C, feed liquid passes through plate and frame filter press, obtains concentration after filters pressing
30%, content of sulfur dioxide 0.01%, solution are in flaxen hydrochloric acid.
Waste hydrochloric acid in the present invention is the formation that the tail gas that Sucralose high-temperature chlorination generates is absorbed with water, is had
The features such as impurity is more, irritation is strong, difficult remove a small amount of sulfide and carbide that high temperature generates by filter press, are stirring
Dropwise addition hydrogen peroxide oxidation sulfide therein in kettle is mixed, temperature reaction, condensate liquid reflux, fixed gas removes tail gas absorption, to reach
To impurity content in aqueous hydrochloric acid solution is reduced, achieve the purpose that edulcoration purification.
The present invention has the advantages that
1) treated hydrochloric acid, purity is higher, and use scope is wider；
2) reduce solid waste, the waste water of HCl treatment than conventional method；
3) process range is wide, and various waste hydrochloric acids can be handled substantially with the method；
4) for production it is normal, continuously run, provide a strong guarantee, solve the trouble and worry of production；
5) processing cost of waste hydrochloric acid is greatly reduced, so that production cost is reduced, so that product profit maximizes；
6) treated hydrochloric acid, can produce chloroethanes, extend the industrial chain of company, provide chloroethene for company's fragrance project
Alkane raw material.
Specific implementation method:
Example one:
Waste hydrochloric acid of the present invention is the formation that the tail gas that Sucralose high-temperature chlorination generates is absorbed with water, concentration 30%
Left and right, content of sulfur dioxide is in 5-10%.Under waste hydrochloric acid room temperature by 20 ㎡ plate and frame filter press remove insoluble impurities carbide,
Waste hydrochloric acid is pressed into the closed enamel still of 5m3 by sulfide, and control waste hydrochloric acid total amount is opened enamel still stirring, be warming up in 3.5m3
45 DEG C, situation in kettle is observed, when bubble-free, the hydrogen peroxide 100L that concentration is 30% is added dropwise, temperature in the kettle is controlled at 50 ± 5 DEG C, directly
When to bubble-free, stop reaction.
Gas phase (gas generated in kettle) pumps to caustic wash tower by the blower of 500 m3/h, 200Pa, uses sodium hydroxide solution
Sulfur dioxide, a small amount of HCl gas in gas phase are absorbed, alkali liquid temperature is controlled at 25 ± 5 DEG C.
Enamel still circulating water cooling is to 20 ± 2 DEG C, and feed liquid passes through 20 ㎡ plate and frame filter press, pressing filtering liquid to hydrochloric acid finished product in kettle
Slot, gained concentration of hydrochloric acid 30% or so, content of sulfur dioxide 0.01%, solution is in faint yellow.
Example two:
Insoluble impurities carbide, sulfide are removed by 20 ㎡ plate and frame filter press under waste hydrochloric acid room temperature, waste hydrochloric acid is pressed into 5m3
Closed enamel still, control waste hydrochloric acid total amount open enamel still stirring, are warming up to 50 DEG C, observe situation in kettle, no gas in 3.5m3
When bubble, the hydrogen peroxide 100L that concentration is 30% is added dropwise, temperature in the kettle is controlled at 50 ± 5 DEG C, until stopping reaction when bubble-free.
Gas phase (gas generated in kettle) pumps to caustic wash tower by the blower of 500 m3/h, 200Pa, uses sodium hydroxide solution
Sulfur dioxide, a small amount of HCl gas in gas phase are absorbed, alkali liquid temperature is controlled at 25 ± 5 DEG C.
Enamel still circulating water cooling is to 20 ± 2 DEG C, and feed liquid passes through 20 ㎡ plate and frame filter press, pressing filtering liquid to hydrochloric acid finished product in kettle
Slot, gained concentration of hydrochloric acid 30% or so, content of sulfur dioxide 0.01%, solution is in faint yellow.
Example three:
Insoluble impurities carbide, sulfide are removed by 20 ㎡ plate and frame filter press under waste hydrochloric acid room temperature, waste hydrochloric acid is pressed into 5m3
Closed enamel still, control waste hydrochloric acid total amount open enamel still stirring, are warming up to 60 DEG C, observe situation in kettle, no gas in 3.5m3
When bubble, the hydrogen peroxide 125L that concentration is 30% is added dropwise, temperature in the kettle is controlled at 50 ± 5 DEG C, until stopping reaction when bubble-free.
Gas phase (gas generated in kettle) pumps to caustic wash tower by the blower of 500 m3/h, 200Pa, uses sodium hydroxide solution
Sulfur dioxide, a small amount of HCl gas in gas phase are absorbed, alkali liquid temperature is controlled at 25 ± 5 DEG C.
Enamel still circulating water cooling is to 20 ± 2 DEG C, and feed liquid passes through 20 ㎡ plate and frame filter press, pressing filtering liquid to hydrochloric acid finished product in kettle
Slot, gained concentration of hydrochloric acid 30% or so, content of sulfur dioxide 0.01%, solution is in faint yellow.
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form；Appoint
What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above
Method and technology contents make many possible changes and modifications to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, anything that does not depart from the technical scheme of the invention according to the technical essence of the invention do above embodiments
Any simple modification, equivalent replacement, equivalence changes and modification, all of which are still within the scope of protection of the technical scheme of the invention.
Claims (1)
1. the waste hydrochloric acid edulcoration purification process in a kind of Sucralose chlorination reaction, including Sucralose high-temperature chlorination step
The tail gas of generation absorbs the waste hydrochloric acid for the concentration 30% to be formed with water, it is characterised in that the following steps are included:
Waste hydrochloric acid removes insoluble impurities carbide, sulfide by plate and frame filter press, and waste hydrochloric acid is then pressed into closed ward off
Porcelain kettle；
Enamel still stirring is opened, is warming up to 45 DEG C -60 DEG C, 30% hydrogen peroxide is added dropwise, temperature is controlled at 50 ± 5 DEG C, until nothing
When bubble, stop reaction；
The gas phase generated in enamel still absorbs sulfur dioxide, HCl gas in gas phase with lye by caustic wash tower；
Through circulating water cooling to 20 ± 5 DEG C, feed liquid passes through plate and frame filter press for feed liquid in enamel still, obtained after filters pressing concentration 30%,
Content of sulfur dioxide 0.01%, solution are in flaxen hydrochloric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811504642.XA CN109607480A (en) | 2018-12-10 | 2018-12-10 | A kind of waste hydrochloric acid edulcoration purification process in Sucralose chlorination reaction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811504642.XA CN109607480A (en) | 2018-12-10 | 2018-12-10 | A kind of waste hydrochloric acid edulcoration purification process in Sucralose chlorination reaction |
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| CN109607480A true CN109607480A (en) | 2019-04-12 |
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| CN201811504642.XA Pending CN109607480A (en) | 2018-12-10 | 2018-12-10 | A kind of waste hydrochloric acid edulcoration purification process in Sucralose chlorination reaction |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105521697A (en) * | 2015-12-08 | 2016-04-27 | 河北科技大学 | Absorbent for removing sulfur dioxide in chloroacetic acid tail gas and removal method |
| CN107890763A (en) * | 2017-11-30 | 2018-04-10 | 成武县晨晖环保科技有限公司 | A kind of chlorinated exhaust absorption process for producing trichloro-acetic chloride |
| CN108751132A (en) * | 2018-07-16 | 2018-11-06 | 南通市常海食品添加剂有限公司 | A kind of sulfur method of Sucralose co-production of hydrochloric |
-
2018
- 2018-12-10 CN CN201811504642.XA patent/CN109607480A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105521697A (en) * | 2015-12-08 | 2016-04-27 | 河北科技大学 | Absorbent for removing sulfur dioxide in chloroacetic acid tail gas and removal method |
| CN107890763A (en) * | 2017-11-30 | 2018-04-10 | 成武县晨晖环保科技有限公司 | A kind of chlorinated exhaust absorption process for producing trichloro-acetic chloride |
| CN108751132A (en) * | 2018-07-16 | 2018-11-06 | 南通市常海食品添加剂有限公司 | A kind of sulfur method of Sucralose co-production of hydrochloric |
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Application publication date: 20190412 |