CN102659647A - Method for producing oxydibenzenesulfonyl hydrazide (OBSH) by using caustic soda replacing ammonia water - Google Patents
Method for producing oxydibenzenesulfonyl hydrazide (OBSH) by using caustic soda replacing ammonia water Download PDFInfo
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- CN102659647A CN102659647A CN2012101219799A CN201210121979A CN102659647A CN 102659647 A CN102659647 A CN 102659647A CN 2012101219799 A CN2012101219799 A CN 2012101219799A CN 201210121979 A CN201210121979 A CN 201210121979A CN 102659647 A CN102659647 A CN 102659647A
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Abstract
The invention relates to a method using caustic soda replacing ammonia water for producing oxydibenzenesulfonyl hydrazide (OBSH), which comprises the steps of firstly adding a double benzene sulfonyl chloride (OBSC), a caustic soda solution and hydrazine hydrate NH2NH2.H2O to a reaction still with a volume of 1L according to mole ratio of OBSC:NaOH:NH2NH2.H2O=1:2:2, stirring continuously, and maintaining the reaction temperature in a range of 20 DEG C to 60 DEG C; stopping stirring after reaction of 3 hours, filtering a product, washing the product to neutral and drying the product in a dryer at the temperature of 60 DEG C; and measuring the quality of the product after drying, calculating the production rate and measuring the decomposition temperature and the gas content. The method has the advantages that ammonia water is replaced with the caustic soda for production, the ammonia nitrogen pollution is eliminated, the quality of the product is not reduced, the production process eliminates ammonia in the product fundamentally, the problem of the ammonia nitrogen pollution is solved completely and the method has great significance for environmental protection.
Description
Technical field
The present invention relates to white whipping agent field, mainly is a kind of method that replaces ammoniacal liquor production OBSH with caustic soda.
Background technology
OBSH (4, the 4-OBSH) is the whiter whipping agent of a kind of use.Its proterties is white fines.150～160 ℃ of decomposition temperatures; Gas forming amount 115～130mL/g, because OBSH decomposition temperature and plastic working temperature comparison match, degradation production is tasteless nontoxic simultaneously, therefore extensively receives the favor of plastic, rubber industry, price is also higher, has good economic benefits.
Traditional technology is produced OBSH and is followed Hydrazine Hydrate 80 and ammoniacal liquor reacted with OBSC, and its reaction equation is: OBSC+2NH
2NH
2H
2O+2NH
3H
2O=OBSH+2NH
4Cl+4H
2O.
This explained hereafter OBSH has the existence of ammonia in its product, cause ammonia and nitrogen pollution easily.The present invention uses sodium hydroxide and replaces the synthetic OBSH of ammoniacal liquor, and its reaction equation is: OBSC+2NH
2NH
2H
2O+2NaOH=OBSH+2NaCl+4H
2O.
Summary of the invention
The object of the invention will overcome the deficiency of above-mentioned technology just, replaces ammoniacal liquor to produce the method for OBSH and provide a kind of with caustic soda.The present invention has fundamentally solved the pollution problem of ammonia nitrogen, and has guaranteed that to a certain extent product quality and productive rate do not descend.
The present invention solves the technical scheme that its technical problem adopts: this method of producing OBSH with caustic soda replacement ammoniacal liquor, and this method comprises following step:
A. at first according to mol ratio OBSC: NaOH: NH
2NH
2H
2O=1: 2: 2 ratio adds OBSC (4, the two benzene sulfonyl chlorides of 4 '-oxo), sodium hydroxide solution and Hydrazine Hydrate 80 NH in the reaction kettle of 1L
2NH
2H
2O, and constantly stir, maintain is at 20 ℃-60 ℃;
B. react and stop after 3 hours stirring, product is filtered, washing is dried in 60 ℃ baking oven to neutral; Temperature of oven should not surpass 70 ℃, with 60 ℃ be the best, prevent the decomposition of the too high OBSH of causing of temperature, influence yield.
C. product quality is measured in the oven dry back, calculates productive rate and measures decomposition temperature and gas forming amount.
As preferably, the purity of used OBSC is 98%.
As preferably, in said step a, used reaction kettle is the reaction kettle that has agitating function or be furnished with whisking appliance.
As preferably, in described step b, the concentration of volume percent of used sodium hydroxide is 5%-50%, excessive concentration, and product is not easy filtration washing, and concentration is low excessively, and water loss is bigger.
The effect that the present invention is useful is: substitute ammoniacal liquor production with caustic soda, eliminate ammonia and nitrogen pollution, and product quality is not descended.The production technique that the present invention studied has fundamentally been eliminated the existence of ammonia in the product, has thoroughly solved the pollution problem of ammonia nitrogen, for environment protection significant meaning is arranged.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with for example.Should be appreciated that described hereinly, and be not used in qualification the present invention for example only in order to explaining the present invention.
This method of producing OBSH of the present invention with caustic soda replacement ammoniacal liquor, this method comprises following step:
A. at first according to mol ratio OBSC: NaOH: NH
2NH
2H
2O=1: 2: 2 ratio adds OBSC (4, the two benzene sulfonyl chlorides of 4 '-oxo), sodium hydroxide solution and Hydrazine Hydrate 80 NH in the reaction kettle of 1L
2NH
2H
2O, and constantly stir, maintain is at 20 ℃-60 ℃;
B. react and stop after 3 hours stirring, product is filtered, washing is dried in 60 ℃ baking oven to neutral; Temperature of oven should not surpass 70 ℃, with 60 ℃ be the best, prevent the decomposition of the too high OBSH of causing of temperature, influence yield.
C. product quality is measured in the oven dry back, calculates productive rate and measures decomposition temperature and gas forming amount.
Embodiment 1
At first in the reaction kettle of 1L, add 22.38gOBSC (purity is 98%), 20mL concentration is 20% sodium hydroxide solution and the Hydrazine Hydrate 80 of 7.6mL80%, and heating makes water temperature remain on 20 ℃, and stirring reaction took out product after 3 hours, filters, and washing is to neutral.Be positioned in 60 ℃ the baking oven and dry.Calculate yield 95.4%.
Embodiment 2
At first in the reaction kettle of 1L, add 10.29g OBSC (purity is 98%), 20mL concentration is 10% sodium hydroxide solution and the Hydrazine Hydrate 80 of 3.5mL80%, and heating makes water temperature remain on 30 ℃, and stirring reaction took out product after 3 hours, filtered, and washing is to neutrality.Be positioned in 60 ℃ the baking oven and dry.Calculate yield 95.9%.
Embodiment 3
At first in the reaction kettle of 1L, add 10.29gOBSC (purity is 98%), 20mL concentration is 10% sodium hydroxide solution and the Hydrazine Hydrate 80 of 3.5mL80%, and heating makes water temperature remain on 40 ℃, and stirring reaction took out product after 3 hours, filters, and washing is to neutral.Be positioned in 60 ℃ the baking oven and dry.Calculate yield 96.4%.
Embodiment 4
At first in the reaction kettle of 1L, add 10.29gOBSC (purity is 98%), 20mL concentration is 10% sodium hydroxide solution and the Hydrazine Hydrate 80 of 3.5mL80%, and heating makes water temperature remain on 60 ℃, and stirring reaction took out product after 3 hours, filters, and washing is to neutral.Be positioned in 60 ℃ the baking oven and dry.Calculate yield 98.4%.
At last, should be pointed out that above instance only is the more representational example of the present invention.Obviously, technical scheme of the present invention is not limited to above-mentioned instance, and many distortion can also be arranged, and all distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (4)
1. one kind replaces ammoniacal liquor to produce the method for OBSH with caustic soda, and it is characterized in that: this method comprises following step:
A. at first according to mol ratio OBSC: NaOH: NH
2NH
2H
20=1: 2: 2 ratio adds OBSC, sodium hydroxide solution and Hydrazine Hydrate 80 NH in the reaction kettle of 1L
2NH
2H
20, and constantly stir, maintain is at 20 ℃-60 ℃;
B. react and stop after 3 hours stirring, product is filtered, be washed to neutrality, in 60 ℃ baking oven, dry;
C. product quality is measured in the oven dry back, calculates productive rate and measures decomposition temperature and gas forming amount.
2. method of producing OBSH with caustic soda replacement ammoniacal liquor according to claim 1, it is characterized in that: the purity of used OBSC is 98%.
3. method of producing OBSH with caustic soda replacement ammoniacal liquor according to claim 1 is characterized in that: in said step a, used reaction kettle is the reaction kettle that has agitating function or be furnished with whisking appliance.
4. method of producing OBSH with caustic soda replacement ammoniacal liquor according to claim 1, it is characterized in that: in described step b, the concentration of volume percent of used sodium hydroxide is 5%-50%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101219799A CN102659647A (en) | 2012-04-24 | 2012-04-24 | Method for producing oxydibenzenesulfonyl hydrazide (OBSH) by using caustic soda replacing ammonia water |
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|---|---|---|---|
| CN2012101219799A CN102659647A (en) | 2012-04-24 | 2012-04-24 | Method for producing oxydibenzenesulfonyl hydrazide (OBSH) by using caustic soda replacing ammonia water |
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| CN102659647A true CN102659647A (en) | 2012-09-12 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588703A (en) * | 2016-10-26 | 2017-04-26 | 山东天化学股份有限公司 | Method for preparing high-purity 4,4'-oxybisbenzensulfonyl chloride |
| CN110194729A (en) * | 2019-06-13 | 2019-09-03 | 台州市前进化工有限公司 | One inter-species nitro-beta-hydroxyethyl sulfuryl preparation method |
| CN114436907A (en) * | 2020-11-03 | 2022-05-06 | 内蒙古锦洋化学工业有限公司 | Environment-friendly preparation method of foaming agent |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2552065A (en) * | 1950-08-01 | 1951-05-08 | Us Rubber Co | Oxybisphenylsulfonhydrazide |
| JPS60156662A (en) * | 1984-01-25 | 1985-08-16 | Eiwa Kasei Kogyo Kk | Preparation of p,p'-oxybis(benzenesulfonyl chloride) |
| CN1105663A (en) * | 1994-02-21 | 1995-07-26 | 苏州化工农药集团公司 | Method for preparing foaming agent 4,4'-para-sulfonyl hydrazine diphenyl ether |
| JP2007262044A (en) * | 2006-03-27 | 2007-10-11 | Eiwa Kasei Kogyo Kk | Method for producing p, p'-oxybis(benzenesulfonyl hydrazide) |
-
2012
- 2012-04-24 CN CN2012101219799A patent/CN102659647A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2552065A (en) * | 1950-08-01 | 1951-05-08 | Us Rubber Co | Oxybisphenylsulfonhydrazide |
| JPS60156662A (en) * | 1984-01-25 | 1985-08-16 | Eiwa Kasei Kogyo Kk | Preparation of p,p'-oxybis(benzenesulfonyl chloride) |
| CN1105663A (en) * | 1994-02-21 | 1995-07-26 | 苏州化工农药集团公司 | Method for preparing foaming agent 4,4'-para-sulfonyl hydrazine diphenyl ether |
| JP2007262044A (en) * | 2006-03-27 | 2007-10-11 | Eiwa Kasei Kogyo Kk | Method for producing p, p'-oxybis(benzenesulfonyl hydrazide) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588703A (en) * | 2016-10-26 | 2017-04-26 | 山东天化学股份有限公司 | Method for preparing high-purity 4,4'-oxybisbenzensulfonyl chloride |
| CN106588703B (en) * | 2016-10-26 | 2018-06-29 | 山东天一化学股份有限公司 | A kind of preparation method of the double benzene sulfonyl chlorides of 4,4 '-oxo of high-purity |
| CN110194729A (en) * | 2019-06-13 | 2019-09-03 | 台州市前进化工有限公司 | One inter-species nitro-beta-hydroxyethyl sulfuryl preparation method |
| CN114436907A (en) * | 2020-11-03 | 2022-05-06 | 内蒙古锦洋化学工业有限公司 | Environment-friendly preparation method of foaming agent |
| KR20220059782A (en) * | 2020-11-03 | 2022-05-10 | 주식회사 금양 | Eco-friendly manufacturing method of foaming agent |
| KR102540597B1 (en) * | 2020-11-03 | 2023-06-12 | 주식회사 금양 | Eco-friendly manufacturing method of foaming agent |
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Application publication date: 20120912 |