CN1459444A - Method of producing sodium formate using crude methyl alcohol rectification residual liquid in production of sodium hydrosulfite - Google Patents
Method of producing sodium formate using crude methyl alcohol rectification residual liquid in production of sodium hydrosulfite Download PDFInfo
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- CN1459444A CN1459444A CN 03112293 CN03112293A CN1459444A CN 1459444 A CN1459444 A CN 1459444A CN 03112293 CN03112293 CN 03112293 CN 03112293 A CN03112293 A CN 03112293A CN 1459444 A CN1459444 A CN 1459444A
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Abstract
A process for preparing sodium formate from the residual liquid generated by rectifying crude methanol in the production of hydros includes such steps as preconcentrating by water vapor at 100-130 deg.C under at least 0.3 MPa, vacuum concentrating at temp. lower than 80 deg.C under 0.05--0.08 MPa, vacuum crystallizing at temp. lower than 90 deg.C under -0.05--0.08 MPa, extracting 50-80 deg.C under -0.05--0.08 MPa, continuously stirring for 10 min, and then clarrifying.
Description
Technical field: the present invention relates to utilize the method that thick methyl alcohol (methanol-water system) distillation residual liquid (hereinafter to be referred as distillation residual liquid) is produced sodium formiate in vat powder (V-Brite B) production process, particularly a kind of method of utilizing distillation residual liquid through explained hereafter sodium formiates such as pre-concentration, vacuum concentration, crystallization extractions.
Background technology: in existing vat powder production process, must add excessive sodium formiate, react the pH value of feed liquid in the 4-5 scope with control, guarantee the stable of reaction system, the quality of Guarantee Insurance powder, this just makes the sodium formiate that contains 60-120g/L in the distillation residual liquid of vat powder production process.Cause material waste and contaminate environment after the discharging.
Summary of the invention: purpose of the present invention is exactly material waste and the problem of environment pollution caused in order to be caused behind the residual liquid discharge that solves the background technology existence.Technical scheme of the present invention is achieved in that a kind of method that thick methanol rectified raffinate is produced sodium formiate in the vat powder production process of utilizing, it is characterized in that this method realizes as follows: (1) pre-concentration: with distillation residual liquid in concentrating 1st effective evaporator, the control liquid level is between two visors, with pressure 〉=0.3MPa water vapor, carry out pre-concentration under 100～130 ℃ of conditions of pre-concentration liquid temp, available midway raffinate is added the liquid level several times, when concentrated solution proportion reached 1.20～1.35g/L, pre-concentration finished; (2), vacuum concentration: open vacuum pump pre-concentration liquid is pumped in the vacuum concentration vaporizer, the control liquid level is between two visors, utilize secondary steam that pre-concentration produces vacuum pressure P=-0.05～-when 0.08MPa, vacuum concentration temperature≤80 ℃, carry out vacuum concentration, can add the liquid level several times with pre-concentration liquid midway, when concentrated solution proportion reached 1.40-1.55g/L, vacuum concentration finished; (3), crystallization extraction: vacuum concentration liquid is put into crystallization extraction pot, open to stir and open the jacket steam valve, vacuum pressure P=-0.05～-0.08MPa, carry out vacuum crystallization during Tc≤90 ℃, when the material crystallization is thick liquid in the pot, use the nitrogen vacuum breaker, add with vacuum concentration liquid volume ratio be that 1/3～3/4 methyl alcohol is in crystallization extraction pot, open and stir, open jacket steam vacuum pressure P=-0.05～-0.08MPa, extraction temperature is to stop to stir behind 50～80 ℃ of conditions continuation stirring 10min sinking clearly, clear liquid in the pot is pressed in the methanol rectification pot with nitrogen, in crystallization extraction pot, add again and vacuum concentration liquid volume ratio is 1/3～3/4 methyl alcohol, repeat above-mentioned extraction process, adding with vacuum concentration liquid volume ratio through the sodium formiate of extraction treatment is 1/3～1/2 methyl alcohol, after fully stirring evenly, be pressed in the four unification moisture eliminators with nitrogen, carry out press filtration, the sodium formiate after pressing dry is through check, send vat powder production batching after the metering.Optimum condition in wherein above each step is: with pressure 0.4MPa water vapor, carry out pre-concentration under 105～120 ℃ of conditions of pre-concentration liquid temp; When concentrated solution proportion reached 1.25～1.30g/L, pre-concentration finished; Utilize secondary steam that pre-concentration produces vacuum pressure P=-0.07～-when 0.08MPa, vacuum concentration temperature≤75 ℃, carry out vacuum concentration; When concentrated solution proportion reached 1.45-1.50g/L, vacuum concentration finished; Vacuum pressure P=-0.07～-carry out vacuum crystallization when 0.08MPa, Tc≤80 ℃; Vacuum pressure P=-0.07～-0.08MPa, extraction temperature be stop to stir after 60～70 ℃ of conditions continue to stir 10min heavy clear.
Embodiment: embodiment 1, this inventive method realize as follows: (1), pre-concentration: add in concentrating 1st effective evaporator, if the supreme visor of 1200L raffinate place, open the steam (valve of P 〉=0.3MPa), control concentrated solution temperature is 105～120 ℃ and carries out pre-concentration, available raffinate fluid infusion position 2 times midway.When the concentrated solution temperature reached 119 ℃, surveying its proportion with the graduated cylinder sampling was 1.30g/L, and pre-concentration finishes; (2), vacuum concentration: open vacuum pump pre-concentration liquid is pumped in the vacuum concentration vaporizer, the control liquid level is between two visors, utilize secondary steam that pre-concentration produces vacuum pressure P=-0.07～-0.08MPa, carry out vacuum concentration during concentrated solution temperature≤80 ℃.Can add liquid level 2 times with pre-concentration liquid midway, surveying its proportion with the graduated cylinder sampling is 1.48g/L, and vacuum concentration finishes; (3), crystallization extraction: vacuum concentration liquid is put into 2 batches in crystallization extraction pot, open and stir, open the jacket steam valve, vacuum pressure P=-0.07～-0.08MPa, carry out vacuum crystallization during temperature≤80 ℃, when the material crystallization is thick liquid in the pot, use the nitrogen vacuum breaker, to join through the 1500L refined methanol of methyl alcohol test tank metering in the crystallization extraction pot, open and stir, open the chuck steam, vacuum pressure P=-0.07～-0.08MPa, temperature is continue to stir under the 60-70 ℃ of condition to stop to stir behind the 10min heavy clear, and clear liquid in the pot is pressed in the methanol rectification pot with nitrogen.In crystallization extraction pot, add 1500L refined methanol again through the metering of methyl alcohol test tank, repeat above-mentioned extraction process, add the 1000L refined methanol to sodium formiate through extraction treatment, after fully stirring evenly, be pressed into four unifications with nitrogen and carry out press filtration in the moisture eliminators, obtaining sodium formiate content after pressing dry is 65.8%, and weight is 568kg, is used for vat powder production batching.
If example 2: this inventive method realizes as follows: (1), pre-concentration: add in concentrating 1st effective evaporator the supreme visor of 1200L raffinate place, open the steam (valve of P 〉=0.3MPa), control concentrated solution temperature is 105～120 ℃ and carries out pre-concentration, available midway raffinate fluid infusion position 3 times, when the concentrated solution temperature reaches 120 ℃, surveying its proportion with the graduated cylinder sampling is 1.28g/L, and pre-concentration finishes; (2), vacuum concentration: open vacuum pump pre-concentration liquid is pumped in the vacuum concentration vaporizer, the control liquid level is between two visors, utilize secondary steam that pre-concentration produces vacuum pressure P=-0.07～-0.08MPa, carry out vacuum concentration during concentrated solution temperature≤80 ℃.Can add liquid level 3 times with pre-concentration liquid midway, surveying its proportion with the graduated cylinder sampling is 1.47g/L, vacuum concentration finishes: (3), crystallization extraction: vacuum concentration liquid is put into 3 batches in crystallization extraction pot, open and stir, open the jacket steam valve, vacuum pressure P=-0.07～-0.08MPa, carry out vacuum crystallization during temperature≤80 ℃, when the material crystallization is thick liquid in the pot, use the nitrogen vacuum breaker, to join through the 1500L refined methanol of methyl alcohol test tank metering in the crystallization extraction pot, open and stir, open jacket steam vacuum pressure P=-0.07～-0.08MPa, temperature is to stop to stir behind the continuation stirring 10min under the 60-70 ℃ of condition sinking clearly, and clear liquid in the pot is pressed into (methyl alcohol after the rectifying is reusable) in the methanol rectification pot with nitrogen.In crystallization extraction pot, add 1500L refined methanol again through the metering of methyl alcohol test tank, repeat above-mentioned extraction process, add the 1200L refined methanol to sodium formiate through extraction treatment, after fully stirring evenly, be pressed into four unifications with nitrogen and carry out press filtration in the moisture eliminators, obtaining sodium formiate content after pressing dry is 62.4%, and weight 645kg is used for vat powder production batching.
Claims (17)
1, a kind of method of utilizing thick methanol rectified raffinate production sodium formiate in the vat powder production process, it is characterized in that this method realizes as follows: (1) pre-concentration: with distillation residual liquid in concentrating 1st effective evaporator, the control liquid level is between two visors, with pressure 〉=0.3MPa water vapor, carry out pre-concentration under 100～130 ℃ of conditions of pre-concentration liquid temp, available midway raffinate is added the liquid level several times, and when concentrated solution proportion reached 1.20～1.35g/L, pre-concentration finished; (2), vacuum concentration: open vacuum pump pre-concentration liquid is pumped in the vacuum concentration vaporizer, the control liquid level is between two visors, utilize secondary steam that pre-concentration produces vacuum pressure P=-0.05～-0.08MPa, during vacuum concentration temperature≤80 ℃, carry out vacuum concentration, can add the liquid level several times with pre-concentration liquid midway, when concentrated solution proportion reaches 1.40-1.55g/L, vacuum concentration finishes: (3), crystallization extraction: vacuum concentration liquid is put into crystallization extraction pot, open to stir and open the jacket steam valve, vacuum pressure P=-0.05～-0.08MPa, carry out vacuum crystallization during Tc≤90 ℃, when the material crystallization is thick liquid in the pot, use the nitrogen vacuum breaker, add with vacuum concentration liquid volume ratio be that 1/3～3/4 methyl alcohol is in crystallization extraction pot, open and stir, open jacket steam vacuum pressure P=-0.05～-0.08MPa, extraction temperature is to stop to stir behind 50～80 ℃ of conditions continuation stirring 10min sinking clearly, clear liquid in the pot is pressed in the methanol rectification pot with nitrogen, in crystallization extraction pot, add again and vacuum concentration liquid volume ratio is 1/3～3/4 methyl alcohol, repeat above-mentioned extraction process, adding with vacuum concentration liquid volume ratio through the sodium formiate of extraction treatment is 1/3～1/2 methyl alcohol, after fully stirring evenly, be pressed in the four unification moisture eliminators with nitrogen, carry out press filtration, the sodium formiate after pressing dry is through check, send vat powder production batching after the metering.
2, according to the described a kind of method that thick methanol rectified raffinate is produced sodium formiate in the vat powder production process of utilizing of claim 1, it is characterized in that water vapor, carry out pre-concentration under 105～120 ℃ of conditions of pre-concentration liquid temp with pressure 0.4MPa.
3, according to claim 1 or 2 described a kind of methods that thick methanol rectified raffinate is produced sodium formiate in the vat powder production process of utilizing, it is characterized in that when concentrated solution proportion reaches 1.25～1.30g/L pre-concentration finishes.
4, according to claim 1 or 2 described a kind of methods that thick methanol rectified raffinate is produced sodium formiate in the vat powder production process of utilizing, it is characterized in that utilizing secondary steam that pre-concentration produces vacuum pressure P=-0.07～-when 0.08MPa, vacuum concentration temperature≤75 ℃, carry out vacuum concentration.
5, according to the described a kind of method that thick methanol rectified raffinate is produced sodium formiate in the vat powder production process of utilizing of claim 3, it is characterized in that utilizing secondary steam that pre-concentration produces vacuum pressure P=-0.07～-when 0.08MPa, vacuum concentration temperature≤75 ℃, carry out vacuum concentration.
6, according to claim 1 or 2 described a kind of methods that thick methanol rectified raffinate is produced sodium formiate in the vat powder production process of utilizing, it is characterized in that when concentrated solution proportion reaches 1.45-1.50g/L vacuum concentration finishes.
7, according to the described a kind of method that thick methanol rectified raffinate is produced sodium formiate in the vat powder production process of utilizing of claim 3, it is characterized in that when concentrated solution proportion reaches 1.45-1.50g/L vacuum concentration finishes.
8, according to the described a kind of method that thick methanol rectified raffinate is produced sodium formiate in the vat powder production process of utilizing of claim 4, it is characterized in that when concentrated solution proportion reaches 1.45-1.50g/L vacuum concentration finishes.
9, describedly a kind ofly utilize in the vat powder production process thick methanol rectified raffinate to produce the methods of sodium formiate according to claim 1 or 2, it is characterized in that vacuum pressure P=-0.07～-carry out vacuum crystallization when 0.08MPa, Tc≤80 ℃.
10, a kind ofly utilize in the vat powder production process thick methanol rectified raffinate to produce the method for sodium formiate according to claim 3 is described, it is characterized in that vacuum pressure P=-0.07～-carry out vacuum crystallization when 0.08MPa, Tc≤80 ℃.
11, a kind ofly utilize in the vat powder production process thick methanol rectified raffinate to produce the method for sodium formiate according to claim 4 is described, it is characterized in that vacuum pressure P=-0.07～-carry out vacuum crystallization when 0.08MPa, Tc≤80 ℃.
12, a kind ofly utilize in the vat powder production process thick methanol rectified raffinate to produce the method for sodium formiate according to claim 6 is described, it is characterized in that vacuum pressure P=-0.07～-carry out vacuum crystallization when 0.08MPa, Tc≤80 ℃.
13, describedly a kind ofly utilize in the vat powder production process thick methanol rectified raffinate to produce the methods of sodium formiate according to claim 1 or 2, it is characterized in that vacuum pressure P=-0.07～-0.08MPa, extraction temperature be stop to stir after 60～70 ℃ of conditions continue to stir 10min heavy clear.
14, a kind ofly utilize in the vat powder production process thick methanol rectified raffinate to produce the method for sodium formiate according to claim 3 is described, it is characterized in that vacuum pressure P=-0.07～-0.08MPa, extraction temperature be stop to stir after 60～70 ℃ of conditions continue to stir 10min heavy clear.
15, a kind ofly utilize in the vat powder production process thick methanol rectified raffinate to produce the method for sodium formiate according to claim 4 is described, it is characterized in that vacuum pressure P=-0.07～-0.08MPa, extraction temperature be stop to stir after 60～70 ℃ of conditions continue to stir 10min heavy clear.
16, a kind ofly utilize in the vat powder production process thick methanol rectified raffinate to produce the method for sodium formiate according to claim 6 is described, it is characterized in that vacuum pressure P=-0.07～-0.08MPa, extraction temperature be stop to stir after 60～70 ℃ of conditions continue to stir 10min heavy clear.
17, a kind ofly utilize in the vat powder production process thick methanol rectified raffinate to produce the method for sodium formiate according to claim 9 is described, it is characterized in that vacuum pressure P=-0.07～-0.08MPa, extraction temperature be stop to stir after 60～70 ℃ of conditions continue to stir 10min heavy clear.
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| CN 03112293 CN1222499C (en) | 2003-05-29 | 2003-05-29 | Method of producing sodium formate using crude methyl alcohol rectification residual liquid in production of sodium hydrosulfite |
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| CN 03112293 CN1222499C (en) | 2003-05-29 | 2003-05-29 | Method of producing sodium formate using crude methyl alcohol rectification residual liquid in production of sodium hydrosulfite |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199417A (en) * | 2010-03-23 | 2011-09-28 | 张以河 | Technology for preparing mineral composite solid lubricant for well drilling on basis of by-products in chemical industry |
| CN102746134A (en) * | 2012-07-13 | 2012-10-24 | 湖南中成化工有限公司 | Method for decreasing content of sodium chloride impurities in recovered sodium formate |
| CN104177248A (en) * | 2014-08-25 | 2014-12-03 | 湖南中成化工有限公司 | Novel treatment technique of sodium hydrosulfite mother solution rectification raffinate |
| CN104341328A (en) * | 2014-10-16 | 2015-02-11 | 烟台市金河保险粉厂有限公司 | Method for producing ethanethiol by utilizing distilled crude methanol residue liquid in production process of sodium hydrosulfite |
| CN113527086A (en) * | 2021-07-30 | 2021-10-22 | 湖北宜化化工股份有限公司 | Method for reducing residue generation amount in sodium hydrosulfite production process |
-
2003
- 2003-05-29 CN CN 03112293 patent/CN1222499C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199417A (en) * | 2010-03-23 | 2011-09-28 | 张以河 | Technology for preparing mineral composite solid lubricant for well drilling on basis of by-products in chemical industry |
| CN102199417B (en) * | 2010-03-23 | 2016-01-20 | 中国地质大学（北京） | One prepares drilling well mineral composite solid lubricating agent technology based on chemical byproduct |
| CN102746134A (en) * | 2012-07-13 | 2012-10-24 | 湖南中成化工有限公司 | Method for decreasing content of sodium chloride impurities in recovered sodium formate |
| CN104177248A (en) * | 2014-08-25 | 2014-12-03 | 湖南中成化工有限公司 | Novel treatment technique of sodium hydrosulfite mother solution rectification raffinate |
| CN104177248B (en) * | 2014-08-25 | 2015-09-09 | 湖南中成化工有限公司 | A kind of distillation residual liquid treatment process of vat powder mother liquor |
| CN104341328A (en) * | 2014-10-16 | 2015-02-11 | 烟台市金河保险粉厂有限公司 | Method for producing ethanethiol by utilizing distilled crude methanol residue liquid in production process of sodium hydrosulfite |
| CN113527086A (en) * | 2021-07-30 | 2021-10-22 | 湖北宜化化工股份有限公司 | Method for reducing residue generation amount in sodium hydrosulfite production process |
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