CN100439257C - Method for treating acid-extracted waste liquid used for production of saccharin sodium - Google Patents
Method for treating acid-extracted waste liquid used for production of saccharin sodium Download PDFInfo
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- CN100439257C CN100439257C CNB200610014743XA CN200610014743A CN100439257C CN 100439257 C CN100439257 C CN 100439257C CN B200610014743X A CNB200610014743X A CN B200610014743XA CN 200610014743 A CN200610014743 A CN 200610014743A CN 100439257 C CN100439257 C CN 100439257C
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Abstract
The present invention discloses a method for processing the acid precipitation waste liquor of saccharin sodium dihydrate. A hydrochloric acid part contained in the waste liquor after acid precipitation is used for replacing sulfuric acid which is used in the original production for directly absorbing ammonia gas exhausted in the procedure of acyl ammoniation, and accordingly, the consumption of the sulfuric acid can be reduced. In addition, a distilling method is adopted to separate methanol from mother liquor containing ammonium chloride, and evaporated liquor comprising the methanol is directly used as hot water used in an esterification procedure to enhance the content of the methanol; finally, the distilling method is used for recovering the methanol and is directly used for the production process of the saccharin sodium dihydrate. The ammonium chloride which is recovered by using the method of evaporation of the mother liquor can be used as a fertiliser and a chemical engineering synthesis raw material, and in this way, useful materials in the acid precipitation waste liquor can be fully used; the environmental pollution can be reduced after the methanol, the ammonium chloride and the hydrochloric acid which are contained in the waste liquor are discharged; in addition, because the processing method can be completed by means of a part of the original production equipment of the saccharin sodium dihydrate, the input of fund can not be greatly increased, and accordingly, the production cost can be reduced.
Description
Technical field
The invention belongs to the synthetic field of chemical industry, particularly relate to a kind of treatment process of acid-extracted waste liquid used for production of saccharin sodium.
Background technology
Usually the soluble saccharin that uses as sweetening agent is the sodium salt of asccharin, soluble in water, its be by water-fast asccharin through amidated, Hofmann degradation fatization, diazotization, displacement, chlorination, ammonification, acid out, alkalization and decoloring reaction and make the soluble saccharin aqueous solution, then this solution is filtered, is concentrated into finite concentration and decrease temperature crystalline, drying and make.Wherein ammonification liquid acid out is gone out to contain in the waste liquid that produces after the saccharin insoluble a spot of hydrochloric acid, 8～12% ammonium chloride and 5% methyl alcohol.This waste water all is in the employing liquid caustic soda and the treatment process of the direct discharging in back at present; and the compound and the organism that wherein can utilize do not reclaimed; so not only can waste resource and increase production cost; and also can cause certain pollution behind this discharging of waste liquid, thereby be unfavorable for environment protection environment.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide and a kind ofly can reclaim useful chemical substance and reduce environmental pollution, and the treatment process of the acid-extracted waste liquid used for production of saccharin sodium that can reduce production costs.
In order to achieve the above object, the treatment process of acid-extracted waste liquid used for production of saccharin sodium provided by the invention comprises the following step that carries out in order:
1) waste liquid behind the ammonification liquid acid out is fed the absorption ammonia that circulates in the ammonia excretion absorption tower and reach 6 until the pH value of waste liquid;
2) will distill in the above-mentioned waste liquid stirring that in the ammonia excretion absorption tower, obtains behind the circulation absorption ammonia, collected volume is the evaporated liquor that contains methyl alcohol of waste liquid amount 50～70% behind the acid out and joins in the esterifier as the used hot water of esterification step, improve the methanol content in this evaporated liquor simultaneously, to distill with distillation tower from the mother liquor that contains methyl alcohol that esterifier is emitted then, collect 64～80 ℃ cut, thereby obtain the methyl alcohol of 70～95% concentration;
3) mother liquor behind the above-mentioned acid out waste liquid distillating carbinol is continued be evaporated to residual volume and reach 40～50% of waste liquid amount behind the acid out, when stirring, add gac and the sodium sulphite that the ratio of waste liquid amount behind weight and the acid out is respectively 1g: 360ml and 1g: 3600ml and carry out deionized and decoloured;
4) mother liquor after deionized and decoloured is filtered, continue then to be evaporated to residual volume reach waste liquid amount behind the acid out 11% after be cooled to 20 ℃ to produce ammonium chloride crystals;
5) mother liquor after the above-mentioned crystallization is filtered to isolate ammonium chloride, then ammonium chloride is carried out drying under 80 ℃ temperature;
6) mother liquor that will isolate ammonium chloride continues reuse.
The described deionized and decoloured time is 20min.
The treatment process of acid-extracted waste liquid used for production of saccharin sodium provided by the invention is that the sulfuric acid that utilizes the salt acid moieties that contains in the waste liquid behind the acid out to replace using in the original production directly absorbs the ammonia of discharging in the amidated operation, thereby can reduce the vitriolic consumption.In addition, adopt the method for evaporation that methyl alcohol is separated with the mother liquor that contains ammonium chloride, and the evaporated liquor that will contain methyl alcohol directly improves its methanol content as the used hot water of esterification step, utilize the distillatory method to reclaim methyl alcohol at last and be directly used in the production process of soluble saccharin, the ammonium chloride that reclaims with the method for mother liquid evaporation then can be used as chemical fertilizer, chemical industry synthesis material, instrument can not make the useful matter in the acid out waste liquid be fully used like this, and can reduce the methyl alcohol, ammonium chloride and the hydrochloric acid that contain in the waste liquid and discharge the pollution of back to environment.In addition, owing to this treatment process can be finished by means of former soluble saccharin part producing equipment, thus can not increase considerably the input of fund, thus can reduce production costs.
Embodiment
Embodiment 1:
1) waste liquid behind the 1800L ammonification liquid acid out is fed the absorption ammonia that circulates in the ammonia excretion absorption tower and reach 6 until the pH value of waste liquid;
2) will distill in the above-mentioned waste liquid stirring that in the ammonia excretion absorption tower, obtains behind the circulation absorption ammonia, collection 1000L contains the evaporated liquor of methyl alcohol and joins in the esterifier as the used hot water of esterification step, improve the methanol content in this evaporated liquor simultaneously, to distill with distillation tower from the mother liquor that contains methyl alcohol that esterifier is emitted then, collect 64～80 ℃ cut, thereby obtain the methyl alcohol of 100L 80% concentration;
3) mother liquor behind the above-mentioned acid out waste liquid distillating carbinol is continued to be evaporated to residual volume and reach 800L, when stirring, add the 5kg gac respectively and 0.5kg sodium sulphite carries out deionized and decoloured 20min;
4) mother liquor after deionized and decoloured is filtered, continue to be evaporated to residual volume then and reach and be cooled to 20 ℃ behind the 200L to produce ammonium chloride crystals;
5) mother liquor after the above-mentioned crystallization is filtered to isolate ammonium chloride, then ammonium chloride is carried out drying under 80 ℃ temperature and obtain the finished product of 150kg;
6) mother liquor that will isolate ammonium chloride continues reuse.
Embodiment 2:
1) waste liquid behind the 1800L ammonification liquid acid out is fed the absorption ammonia that circulates in the ammonia excretion absorption tower and reach 6 until the pH value of waste liquid;
2) will distill in the above-mentioned waste liquid stirring that in the ammonia excretion absorption tower, obtains behind the circulation absorption ammonia, collection 1100L contains the evaporated liquor of methyl alcohol and joins in the esterifier as the used hot water of esterification step, improve the methanol content in this evaporated liquor simultaneously, to distill with distillation tower from the mother liquor that contains methyl alcohol that esterifier is emitted then, collect 64～80 ℃ cut, thereby obtain the methyl alcohol of 105L 80% concentration;
3) mother liquor behind the above-mentioned acid out waste liquid distillating carbinol is continued to be evaporated to residual volume and reach 800L, when stirring, add the 5kg gac respectively and 0.5kg sodium sulphite carries out deionized and decoloured 20min;
4) mother liquor after deionized and decoloured is filtered, continue to be evaporated to residual volume then and reach and be cooled to 20 ℃ behind the 200L to produce ammonium chloride crystals;
5) mother liquor after the above-mentioned crystallization is filtered to isolate ammonium chloride, then ammonium chloride is carried out drying under 80 ℃ temperature and obtain the finished product of 150kg;
6) mother liquor that will isolate ammonium chloride continues reuse.
Embodiment 3:
1) waste liquid behind the 1800L ammonification liquid acid out is fed the absorption ammonia that circulates in the ammonia excretion absorption tower and reach 6 until the pH value of waste liquid;
2) will distill in the above-mentioned waste liquid stirring that in the ammonia excretion absorption tower, obtains behind the circulation absorption ammonia, collection 1050L contains the evaporated liquor of methyl alcohol and joins in the esterifier as the used hot water of esterification step, improve the methanol content in this evaporated liquor simultaneously, to distill with distillation tower from the mother liquor that contains methyl alcohol that esterifier is emitted then, collect 64～80 ℃ cut, thereby obtain the methyl alcohol of 102.5L80% concentration;
3) mother liquor behind the above-mentioned acid out waste liquid distillating carbinol is continued to be evaporated to residual volume and reach 800L, when stirring, add the 5kg gac respectively and 0.5kg sodium sulphite carries out deionized and decoloured 20min;
4) mother liquor after deionized and decoloured is filtered, continue to be evaporated to residual volume then and reach and be cooled to 20 ℃ behind the 200L to produce ammonium chloride crystals;
5) mother liquor after the above-mentioned crystallization is filtered to isolate ammonium chloride, then ammonium chloride is carried out drying under 80 ℃ temperature and obtain the finished product of 150kg;
6) mother liquor that will isolate ammonium chloride continues reuse.
Claims (2)
1, a kind of treatment process of acid-extracted waste liquid used for production of saccharin sodium is characterized in that: the treatment process of described acid-extracted waste liquid used for production of saccharin sodium comprises the following step that carries out in order:
1) waste liquid behind the ammonification liquid acid out is fed the absorption ammonia that circulates in the ammonia excretion absorption tower and reach 6 until the pH of waste liquid value;
2) will distill in the above-mentioned waste liquid stirring that in the ammonia excretion absorption tower, obtains behind the circulation absorption ammonia, collected volume is the evaporated liquor that contains methyl alcohol of waste liquid amount 50～70% behind the acid out and joins in the esterifier as the used hot water of esterification step, improve the methanol content in this evaporated liquor simultaneously, to distill with distillation tower from the mother liquor that contains methyl alcohol that esterifier is emitted then, collect 64～80 ℃ cut, thereby obtain the methyl alcohol of 70～95% concentration;
3) mother liquor behind the above-mentioned acid out waste liquid distillating carbinol is continued be evaporated to residual volume and reach 40～50% of waste liquid amount behind the acid out, when stirring, add gac and the sodium sulphite that the ratio of waste liquid amount behind weight and the acid out is respectively 1g: 360ml and 1g: 3600ml and carry out deionized and decoloured;
4) mother liquor after deionized and decoloured is filtered, continue then to be evaporated to residual volume reach waste liquid amount behind the acid out 11% after be cooled to 20 ℃ to produce ammonium chloride crystals;
5) mother liquor after the above-mentioned crystallization is filtered to isolate ammonium chloride, then ammonium chloride is carried out drying under 80 ℃ temperature;
6) mother liquor that will isolate ammonium chloride continues reuse.
2, the treatment process of acid-extracted waste liquid used for production of saccharin sodium according to claim 1 is characterized in that: the described deionized and decoloured time is 20min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610014743XA CN100439257C (en) | 2006-07-10 | 2006-07-10 | Method for treating acid-extracted waste liquid used for production of saccharin sodium |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610014743XA CN100439257C (en) | 2006-07-10 | 2006-07-10 | Method for treating acid-extracted waste liquid used for production of saccharin sodium |
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| CN1884121A CN1884121A (en) | 2006-12-27 |
| CN100439257C true CN100439257C (en) | 2008-12-03 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106865882B (en) * | 2015-12-13 | 2020-11-27 | 中国科学院大连化学物理研究所 | Method for treating saccharin sodium production wastewater by phthalic anhydride method |
| CN108249460A (en) * | 2018-01-13 | 2018-07-06 | 安徽金禾实业股份有限公司 | In a kind of Sucralose and the processing method of press filtration workshop section ammonium chloride waste residue |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141888A (en) * | 1996-04-11 | 1997-02-05 | 刘立华 | Method for treatment of waste acid liquid containing copper production of gluside and sodium saccharin |
| CN1158320A (en) * | 1996-02-29 | 1997-09-03 | 本溪市环境科学研究所 | Method for reclaiming waste keto-acid liquid in prodn. of soluble gluside |
| CN1541955A (en) * | 2003-11-06 | 2004-11-03 | 上海交通大学 | Recovery and utilization method for copper bearing spent acid solution from sodium saccharin production process |
| CN1663429A (en) * | 2005-03-22 | 2005-09-07 | 天津北方食品有限公司 | Method for producing saccharin sodium |
-
2006
- 2006-07-10 CN CNB200610014743XA patent/CN100439257C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1158320A (en) * | 1996-02-29 | 1997-09-03 | 本溪市环境科学研究所 | Method for reclaiming waste keto-acid liquid in prodn. of soluble gluside |
| CN1141888A (en) * | 1996-04-11 | 1997-02-05 | 刘立华 | Method for treatment of waste acid liquid containing copper production of gluside and sodium saccharin |
| CN1541955A (en) * | 2003-11-06 | 2004-11-03 | 上海交通大学 | Recovery and utilization method for copper bearing spent acid solution from sodium saccharin production process |
| CN1663429A (en) * | 2005-03-22 | 2005-09-07 | 天津北方食品有限公司 | Method for producing saccharin sodium |
Non-Patent Citations (4)
| Title |
|---|
| 糖精生产废液的综合利用. 梅荣武，余劲松，陈芸.化工环保，第18卷第4期. 1998 |
| 糖精生产废液的综合利用. 梅荣武，余劲松，陈芸.化工环保，第18卷第4期. 1998 * |
| 糖精钠的清洁生产. 施剑波.精细与专用化学品，第11期. 2003 |
| 糖精钠的清洁生产. 施剑波.精细与专用化学品，第11期. 2003 * |
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| CN1884121A (en) | 2006-12-27 |
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Assignee: Tianjin tiannu Chemical Industry Group Co. Assignor: Tianjin Beifang Food Co., Ltd. Contract fulfillment period: 2009.7.30 to 2014.7.29 contract change Contract record no.: 2009120000247 Denomination of invention: Method for treating acid-extracted waste liquid used for production of saccharin sodium Granted publication date: 20081203 License type: Exclusive license Record date: 20091022 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.7.30 TO 2014.7.29; CHANGE OF CONTRACT Name of requester: TIANJIN TIANNV CHEMICAL INDUSTRIAL GROUP CO., LTD. Effective date: 20091022 |