CN106336365A - Production process of electroplating grade methanesulfonic acid - Google Patents
Production process of electroplating grade methanesulfonic acid Download PDFInfo
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- CN106336365A CN106336365A CN201610732707.0A CN201610732707A CN106336365A CN 106336365 A CN106336365 A CN 106336365A CN 201610732707 A CN201610732707 A CN 201610732707A CN 106336365 A CN106336365 A CN 106336365A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/16—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by oxidation of thiols, sulfides, hydropolysulfides, or polysulfides with formation of sulfo or halosulfonyl groups
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of electroplating chemicals, and relates to a production technology of electroplating grade methanesulfonic acid. The technology includes the following steps of adding dimethyl disulfide and deionized water into a reaction still to be evenly stirred, introducing chlorine to prepare methylsufonyl chloride, conducting standing still and layering to introduce the lower layer material into a refining tower, conducting negative pressure refining on the material in the refining tower to obtain methylsufonyl chloride, injecting methylsufonyl chloride into a metering tank, injecting the deionized water into a hydrolysis kettle, dropwise adding methylsufonyl chloride into the hydrolysis kettle for hydrolysis reaction, and obtaining electroplating grade methanesulfonic acid after reaction ends. Compared with the prior art, the technology has the advantages that the technology is simple in process, high in product purity and suitable for electroplating grade; a by-product HCl in reaction is sold, and energy saving and environment protecting are achieved.
Description
Technical field
The invention belongs to electronics finishing field of chemicals, it is related to a kind of production technology of electronics finishing level pyrovinic acid.
Background technology
In recent years, pyrovinic acid electroplate liquid is widely used, the corrosion to base material and equipment for the pyrovinic acid electroplate liquid
Property little, lower than the toxicity of fluoboric acid and fluosilicic acid, plating solution produce waste few, there is biodegradability, bath stability is good, sink
Long-pending speed is fast, and can co-deposit with various metals, and the advantages of alloying component proportion is larger, thus pyrovinic acid electroplate liquid exists
Environmental protection aspect has obvious advantage, it has also become current research and the focus applied.
The demand of the pyrovinic acid of high-quality is more come also greatly, especially to need the electronics finishing field of high-quality.At present
The producer producing pyrovinic acid using DMDS oxidizing process is many, but the highly purified pyrovinic acid of production is relatively fewer, because
And the demand in market can not be met.
Content of the invention
For the above-mentioned problems in the prior art, the present invention proposes a kind of production of electronics finishing level pyrovinic acid
Technique, is carried out as follows:
Step a: DMDS and deionized water 1:0.8～1.2 in mass ratio are added reactor, opens circulating pump, by chlorine
Gas is at the uniform velocity passed through reactor, and the mass ratio of DMDS and chlorine is 1:3.5～5.5, and controlling reaction temperature is 16～22 DEG C,
Reaction time 6～10h, first stops chlorine, closes circulating pump afterwards, after stratification, lower floor's material is passed through rectifying still；
Step b: the material being passed through in step a in rectifying still is carried out negative pressure rectifying, reflux ratio is 2～4；Control pressure be-
During 0.07mpa to -0.08mpa, collect the cut that temperature is 92～98 DEG C；
Step c: the cut that rectifying in step b is obtained, that is, methylsufonyl chloride injection measuring tank, injects deionization in hydrolysis kettle
Water, to 60～70 DEG C, before reaction starts, in methylsufonyl chloride and hydrolysis kettle in measuring tank, the mass ratio of deionized water is heating water
1:0.4～0.8；Methylsufonyl chloride is added drop-wise to hydrolysis kettle, during dropping, controls 70～90 DEG C of solution temperature in hydrolysis kettle, pressure
Power is -4.5kpa～-5.5kpa, reaction time 6～10h, and the preserving heat after reaction ends time is more than 2.5 hours.
Using technique scheme the present invention compared with prior art, process is simple, product purity high it is adaptable to electronics
Plating level, sells outside the accessory substance hcl in reaction, energy-conserving and environment-protective.
Further, the prioritization scheme of the present invention is:
In step a, the mass ratio of DMDS and water is 1:0.9～1.1.
The DMDS putting in step a and the mass ratio of chlorine are 1:4～5.
Reactor outer wall is provided with chuck, is connected with cool brine in chuck, and controlling reaction temperature is 18～20 DEG C.
Rectifying in step b: when controlling pressure for -0.07mpa, a cut, < 95 DEG C of rectification temperature；Two cuts, rectifying temperature
Spend for 95～98 DEG C；Three cuts, rectification temperature > 98 DEG C；Obtain three kinds of cuts are stored for future use respectively.
The reflux ratio controlling rectifying in step b is 2.5～3.5.
The mass ratio that in step c, reaction starts deionized water in methylsufonyl chloride and hydrolysis kettle in front measuring tank is 1:0.5
～0.7.
Control 75～85 DEG C of hydrolysis kettle temperature during dripping in step c.
After in step c, hydrolysis terminates, temperature retention time is 2.8～3.2h.
When controlling pressure for -0.07mpa, collect the cut that temperature is 92～98 DEG C.
Brief description
The process chart of Fig. 1: the present invention.
Specific embodiment
Embodiment 1
The preparation of step a. methylsufonyl chloride
5000l enamel reaction still add 1.5t DMDS, deionized water 1.6t, open cycle pump (centrifugal pump), make from
Sub- water and DMDS mix, and liquid chlorine, after vaporizer gasification, is passed through reactor by reactor bottom, chlorine flow velocity is
0.75t/h, reaction is carried out in reactor full section, one section of packing section of this reactor top setting, can increase response area,
So that the chlorine being passed through fully is reacted, and then improve feed stock conversion.
Reactor outer wall is provided with chuck, is connected with cool brine in chuck, and reaction temperature controls 19 DEG C about, reacts 8 hours, first
Stop chlorine, circulating pump (centrifugal pump) about circulates 20 minutes and stops, reaction end obtains methylsufonyl chloride and unreacted water-soluble
Liquid.Standing a period of time, layering occurs in reactor, lower floor's material enters rectifying still by bottom, and in reactor, upper solution is straight
Connect for next circular response, continue to participate in the preparation of methylsufonyl chloride.
The purification of step b. methylsufonyl chloride
Negative pressure rectifying, Stress control -0.07mpa are adopted to the material entering rectifying column, point three kinds of cuts are collected: one evaporates
Point, rectification temperature < 95 DEG C, mainly contains a small amount of water, unreacted completely DMDS and the micro methyl carried secretly
Sulfonic acid chloride；Two cuts, rectification temperature is 95～98 DEG C, and reflux ratio controls 2.5～3.5,95 DEG C≤bis- cut≤98 DEG C, two cuts
For methylsufonyl chloride；Three cuts, rectification temperature > 98 DEG C, the micro sulfonic acid containing methylsufonyl chloride.Purification stage of rectification, collects
Methylsufonyl chloride 3.45t, methylsufonyl chloride yield 94.5%.
Three kinds of cuts are stored respectively standby, a cut is used for methylsufonyl chloride synthetic reaction, two cuts are used for methyl sulphur
The production of acid, three cuts are used for producing technical grade tin plate sulfonic acid.All cuts are all rationally utilized, and no discarded object produces.
The preparation of step c. pyrovinic acid
By two cut methylsufonyl chloride injection measuring tank in step b, add deionized water 1.5t in the enamel hydrolysis kettle of 5000l,
(opening stirring) chuck leads to steam, is heated deionized water using steam, open cycle pump (centrifugal pump), so that deionized water is heated all
Even, it is heated to 65 DEG C.The methylsufonyl chloride of measuring tank is added drop-wise to hydrolytic reaction pot, micro-negative pressure operation, pressure is about -5kpa,
Methylsufonyl chloride dropping flow velocity is about 0.45t/h, needs rule of thumb to coordinate to adjust steam and rate of addition, prevents bumping, drip
About 7～8h between the added-time, during reaction, strict temperature control is 75～85 DEG C, to completion of dropwise addition, is incubated 3 hours.Produce in course of reaction
Raw hcl adopts three-level falling film absorption, sells outside the by-product hydrochloric acid obtaining of production.
Sample analysis, oxidable thing < 20 ppm, color number (apha) < 20, so42-< 30 ppm, cl-< 5ppm, fe < 5ppm,
Reach the standard of electronics finishing needs, methylsufonyl chloride hydrolyzes conversion ratio 97.8%.
Embodiment 2
The preparation of step a. methylsufonyl chloride
Add deionized water 1t, DMDS 1t, open cycle pump (centrifugal pump) in 3000l enamel reaction still, make deionized water
Mix with DMDS；Liquid chlorine, after gasifier gasification, enters chlorinating container, chlorine flow velocity by reactor bottom
For 0.54t/h, react and carry out in reactor full section, one section of packing section of this reactor top setting, reaction surface can be increased
Long-pending, so that the chlorine being passed through fully is reacted, and then improve feed stock conversion.
Reactor outer wall is provided with chuck, and chuck is passed through cool brine, controls 19 DEG C about of temperature of reaction kettle, reaction time
7.5h, stops chlorine, and circulating pump (centrifugal pump) cuts out after circulating 20 minutes, and reaction end obtains methylsufonyl chloride and unreacted water
Solution.Standing a period of time, layering occurs in reactor, lower floor's material enters rectifying still by bottom, upper solution in reactor
It is directly used in next circular response, continue to participate in the preparation of methylsufonyl chloride.
The purification of step b. methylsufonyl chloride
Negative pressure rectifying, Stress control -0.07mpa are adopted to the material entering rectifying still, point three kinds of cuts are collected: one evaporates
Point, rectification temperature < 95 DEG C, mainly contains a small amount of water, unreacted completely DMDS and the micro methyl carried secretly
Sulfonic acid chloride；Two cuts, rectification temperature is 95～98 DEG C, and reflux ratio controls 2.5～3.0,95 DEG C≤bis- cut≤98 DEG C, two cuts
For methylsufonyl chloride；Three cuts, rectification temperature > 98 DEG C, the micro sulfonic acid containing methylsufonyl chloride.Purification stage of rectification, collects
Methylsufonyl chloride 2.12t, methylsufonyl chloride yield 95.7%.
Three kinds of cuts that rectifying is obtained store respectively standby, a cut be used for methylsufonyl chloride synthetic reaction, two cuts
For the production of pyrovinic acid, three cuts are used for producing technical grade tin plate sulfonic acid.All cuts are all rationally utilized, no useless
Gurry produces.
The preparation of step c. pyrovinic acid
The methylsufonyl chloride that rectifying in step b is obtained injects measuring tank, adds deionized water in the enamel hydrolysis kettle of 3000l
1.2t, chuck leads to steam, is heated deionized water using steam, open cycle pump (centrifugal pump), so that deionized water is heated evenly, plus
Heat is to 65 DEG C；The methylsufonyl chloride of measuring tank is added drop-wise to hydrolytic reaction pot, micro-negative pressure operation, pressure is about -5kpa, methyl sulphur
Acyl chlorides dropping flow velocity is about 0.30t/h, needs rule of thumb to coordinate to adjust steam and rate of addition, prevents bumping, time for adding
About 7～8h, 75～85 DEG C of temperature control during reaction, to completion of dropwise addition, it is incubated 3 hours.The hcl producing in course of reaction adopts three
Level falling film absorption, sells outside the by-product hydrochloric acid of production.
Sample analysis, oxidable thing < 20 ppm, color number (apha) < 20, so42-< 30 ppm, cl-< 5ppm, fe < 5ppm,
Reach the standard of electronics finishing needs, methylsufonyl chloride hydrolyzes conversion ratio 98.3%.
Embodiment 3
The preparation of step a. methylsufonyl chloride
5000l enamel reaction still add 1.6t DMDS, deionized water 1.6t, open cycle pump (centrifugal pump), make from
Sub- water and DMDS mix, and liquid chlorine, after vaporizer gasification, is passed through reactor by reactor bottom, chlorine flow velocity is
0.80t/h, reaction is carried out in reactor full section, one section of packing section of this reactor top setting, can increase response area,
So that the chlorine being passed through fully is reacted, and then improve feed stock conversion.
Reactor outer wall is provided with chuck, is connected with cool brine in chuck, and reaction temperature controls 20 DEG C about, reacts 8 hours, stops
Chlorine, circulating pump (centrifugal pump) stops after circulating 20 minutes again, and reaction end obtains methylsufonyl chloride and the unreacted aqueous solution.Quiet
Put and layering occurs in a period of time, reactor, lower floor's material enters rectifying still by bottom, and in reactor, upper solution is directly used in
Next circular response, continues to participate in the preparation of methylsufonyl chloride.
The purification of step b. methylsufonyl chloride
Negative pressure rectifying, Stress control -0.08mpa are adopted to the material entering rectifying still, point three kinds of cuts are collected: one evaporates
Point, rectification temperature < 92 DEG C, mainly contains a small amount of water, unreacted completely DMDS and the micro methyl carried secretly
Sulfonic acid chloride；Two cuts, rectification temperature is 92～95 DEG C, and reflux ratio controls 2.5～3.0,92 DEG C≤bis- cut≤95 DEG C, two cuts
For methylsufonyl chloride；Three cuts, rectification temperature > 95 DEG C, the micro sulfonic acid containing methylsufonyl chloride.Purification stage of rectification, collects
Methylsufonyl chloride 3.62t, methylsufonyl chloride yield 93.0%.
Three kinds of cuts that rectifying is obtained store respectively standby, a cut be used for methylsufonyl chloride synthetic reaction, two cuts
For the production of pyrovinic acid, three cuts are used for producing technical grade tin plate sulfonic acid.All cuts are all rationally utilized, no useless
Gurry produces.
The preparation of step c. pyrovinic acid
The methylsufonyl chloride that rectifying in step b is obtained injects measuring tank, adds deionized water in the enamel hydrolysis kettle of 5000l
1.8t, chuck leads to steam, is heated deionized water using steam, open cycle pump (centrifugal pump), so that deionized water is heated evenly, plus
Heat is to 70 DEG C；The methylsufonyl chloride of measuring tank is added drop-wise to hydrolytic reaction pot, micro-negative pressure operation, pressure is about -5kpa, methyl sulphur
Acyl chlorides dropping flow velocity is about 0.48t/h, needs rule of thumb to coordinate to adjust steam and rate of addition, prevents bumping, time for adding
About 7～8h, during reaction, strict temperature control is 80～85 DEG C, to completion of dropwise addition, is incubated 3 hours.The hcl producing in course of reaction
Using three-level falling film absorption, produce and sell outside the raw hydrochloric acid of by-product.
Sample analysis, oxidable thing < 20 ppm, color number (apha) < 20, so42-< 30 ppm, cl-< 5ppm, fe < 5ppm,
Reach the standard of electronics finishing needs, methylsufonyl chloride hydrolyzes conversion ratio 96.5%.
Embodiment 4
The preparation of step a. methylsufonyl chloride
3000l enamel reaction still add 1.1t DMDS, deionized water 1.2t, open cycle pump (centrifugal pump), make from
Sub- water and DMDS mix, and liquid chlorine, after vaporizer gasification, is passed through reactor by reactor bottom, chlorine flow velocity is
0.55t/h, reaction is carried out in reactor full section, one section of packing section of this reactor top setting, can increase response area,
So that the chlorine being passed through fully is reacted, and then improve feed stock conversion.
Reactor outer wall is provided with chuck, is connected with cool brine in chuck, and reaction temperature controls 19 DEG C about, and reaction 7 ~ 7.5 is little
When, stop chlorine, circulating pump (centrifugal pump) circulation stops for 20 minutes again, reaction end obtains methylsufonyl chloride and unreacted water-soluble
Liquid.Standing a period of time, layering occurs in reactor, lower floor's material enters rectifying still by bottom, and in reactor, upper solution is straight
Connect for next circular response, continue to participate in the preparation of methylsufonyl chloride.
The purification of step b. methylsufonyl chloride
Negative pressure rectifying, Stress control -0.07mpa are adopted to the material entering rectifying still, point three kinds of cuts are collected: one evaporates
Point, rectification temperature < 95 DEG C, mainly contains a small amount of water, unreacted completely DMDS and the micro methyl carried secretly
Sulfonic acid chloride；Two cuts, rectification temperature is 95～98 DEG C, and reflux ratio controls 2.5 ~ 3.5,95 DEG C≤bis- cut≤98 DEG C, two cuts
For methylsufonyl chloride；Three cuts, rectification temperature > 98 DEG C, the micro sulfonic acid containing methylsufonyl chloride.Purification stage of rectification, collects
Two cut 2.56t, methylsufonyl chloride yield 96.4%.
Three kinds of cuts that rectifying is obtained store respectively standby, a cut be used for methylsufonyl chloride synthetic reaction, two cuts
For the production of pyrovinic acid, three cuts are used for producing technical grade tin plate sulfonic acid.All cuts are all rationally utilized, no useless
Gurry produces.
The preparation of step c. pyrovinic acid
The methylsufonyl chloride that rectifying in step b is obtained injects measuring tank, adds deionized water in the enamel hydrolysis kettle of 3000l
1.2t, chuck leads to steam, is heated deionized water using steam, open cycle pump (centrifugal pump), so that deionized water is heated evenly, water
It is heated to 70 DEG C；The methylsufonyl chloride of measuring tank is added drop-wise to hydrolytic reaction pot, micro-negative pressure operation, pressure is about -5kpa, methyl
Sulfonic acid chloride dropping flow velocity is about 0.34t/h, needs rule of thumb to coordinate to adjust steam and rate of addition, prevents bumping, during dropping
Between about 7～8h, during reaction, strict temperature control is 75～85 DEG C, to completion of dropwise addition, is incubated 3 hours.Produce in course of reaction
Hcl adopts three-level falling film absorption, and the by-product hydrochloric acid obtaining of production is used for selling outward.
Sample analysis, oxidable thing < 20 ppm, color number (apha) < 20, so42-< 30 ppm, cl-< 5ppm, fe < 5ppm,
Reach the standard of electronics finishing needs, methylsufonyl chloride hydrolyzes conversion ratio 98.4%.
Embodiment 5
The preparation of step a. methylsufonyl chloride
5000l enamel reaction still add 1.7t DMDS, deionized water 1.7t, open cycle pump (centrifugal pump), make from
Sub- water and DMDS mix, and liquid chlorine, after vaporizer gasification, is passed through reactor by reactor bottom, chlorine flow velocity is
0.80t/h, reaction is carried out in reactor full section, one section of packing section of this reactor top setting, can increase response area,
So that the chlorine being passed through fully is reacted, and then improve feed stock conversion.
Reactor outer wall is provided with chuck, is connected with cool brine in chuck, and reaction temperature controls 19 DEG C about, reacts 9 hours, stops
Chlorine, circulating pump (centrifugal pump) circulation stops for 20 minutes again, and reaction end obtains methylsufonyl chloride and the unreacted aqueous solution.Standing
For a period of time, layering occurs in reactor, lower floor's material enters rectifying still by bottom, and in reactor, upper solution is directly used in down
One circular response, continues to participate in the preparation of methylsufonyl chloride.
The purification of step b. methylsufonyl chloride
The methylsufonyl chloride entering rectifying still adopts negative pressure rectifying, Stress control -0.07mpa, and point three kinds of cuts are collected: one
One cut, rectification temperature < 95 DEG C, mainly contain a small amount of water, unreacted completely DMDS and carry secretly micro
Methylsufonyl chloride；Two cuts, rectification temperature is 95～98 DEG C, 2.5 ~ 3.0,95 DEG C≤bis- cut≤98 DEG C of reflux ratio control, two
Cut is methylsufonyl chloride；Three cuts, rectification temperature > 98 DEG C, the micro sulfonic acid containing methylsufonyl chloride.Purification stage of rectification,
Collect two cut 3.81t, methylsufonyl chloride yield 92.1%.
Three kinds of cuts that rectifying is obtained store respectively standby, a cut be used for methylsufonyl chloride synthetic reaction, two cuts
For the production of pyrovinic acid, three cuts are used for producing technical grade tin plate sulfonic acid.All cuts are all rationally utilized, no useless
Gurry produces.
The preparation of step c. pyrovinic acid
The methylsufonyl chloride that rectifying in step b is obtained injects measuring tank, adds deionized water in the enamel hydrolysis kettle of 5000l
1.8t, chuck leads to steam, is heated deionized water using steam, open cycle pump (centrifugal pump), so that deionized water is heated evenly, water
It is heated to 70 DEG C；The methylsufonyl chloride of measuring tank is added drop-wise to hydrolytic reaction pot, micro-negative pressure operation, pressure is about -5kpa, methyl
Sulfonic acid chloride dropping flow velocity is about 0.43t/h, needs rule of thumb to coordinate to adjust steam and rate of addition, prevents bumping, during dropping
Between about 8.5 ~ 9.5h, during reaction, strict temperature control is 85～90 DEG C, to completion of dropwise addition, is incubated 3 hours.Produce in course of reaction
Hcl adopt three-level falling film absorption, the by-product hydrochloric acid obtaining of production is used for selling outward or producing for other using.
Sample analysis, oxidable thing < 20 ppm, color number (apha) < 20, so42-< 30 ppm, cl-< 5ppm, fe < 5ppm,
Reach the standard of electronics finishing needs, methylsufonyl chloride hydrolyzes conversion ratio 95.6%.
Claims (10)
1. a kind of production technology of electronics finishing level pyrovinic acid is it is characterised in that carry out as follows:
Step a: DMDS and deionized water 1:0.8～1.2 in mass ratio are added reactor, opens circulating pump, by chlorine
Gas is at the uniform velocity passed through reactor, and the mass ratio of DMDS and chlorine is 1:3.5～5.5, and controlling reaction temperature is 16～22 DEG C,
Reaction time 6～10h, first stops chlorine, closes circulating pump afterwards, after stratification, lower floor's material is passed through rectifying still；
Step b: the material being passed through in step a in rectifying still is carried out negative pressure rectifying, reflux ratio is 2～4；Control pressure be-
During 0.07mpa to -0.08mpa, collect the cut that temperature is 92～98 DEG C；
Step c: the cut that rectifying in step b is obtained, that is, methylsufonyl chloride injection measuring tank, injects deionization in hydrolysis kettle
Water, to 60～70 DEG C, before reaction starts, in methylsufonyl chloride and hydrolysis kettle in measuring tank, the mass ratio of deionized water is heating water
1:0.4～0.8；Methylsufonyl chloride is added drop-wise to hydrolysis kettle, during dropping, controls 70～90 DEG C of solution temperature in hydrolysis kettle, pressure
Power is -4.5kpa～-5.5kpa, reaction time 6～10h, and the preserving heat after reaction ends time is more than 2.5 hours.
2. electronics finishing level pyrovinic acid according to claim 1 production technology it is characterised in that: diformazan in step a
The mass ratio of base two sulphur and water is 1:0.9～1.1.
3. electronics finishing level pyrovinic acid according to claim 1 production technology it is characterised in that: in step a put into
DMDS and chlorine mass ratio be 1:4～5.
4. electronics finishing level pyrovinic acid according to claim 1 production technology it is characterised in that: reactor outer wall sets
There is chuck, in chuck, be connected with cool brine, controlling reaction temperature is 18～20 DEG C.
5. electronics finishing level pyrovinic acid according to claim 1 production technology it is characterised in that: the essence in step b
Evaporate: when controlling pressure for -0.07mpa, a cut, < 95 DEG C of rectification temperature；Two cuts, rectification temperature is 95～98 DEG C；Three evaporate
Point, rectification temperature > 98 DEG C；Obtain three kinds of cuts are stored for future use respectively.
6. electronics finishing level pyrovinic acid according to claim 1 production technology it is characterised in that: in step b control
The reflux ratio of rectifying is 2.5～3.5.
7. electronics finishing level pyrovinic acid according to claim 1 production technology it is characterised in that: in step c react
In methylsufonyl chloride and hydrolysis kettle in measuring tank before beginning, the mass ratio of deionized water is 1:0.5～0.7.
8. electronics finishing level pyrovinic acid according to claim 1 production technology it is characterised in that: in step c drip
During control 75～85 DEG C of hydrolysis kettle temperature.
9. electronics finishing level pyrovinic acid according to claim 1 production technology it is characterised in that: in step c hydrolyze
After reaction terminates, temperature retention time is 2.8～3.2h.
10. electronics finishing level pyrovinic acid according to claim 1 production technology it is characterised in that: control pressure be-
During 0.07mpa, collect the cut that temperature is 92～98 DEG C.
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| CN201610732707.0A CN106336365A (en) | 2016-08-27 | 2016-08-27 | Production process of electroplating grade methanesulfonic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114247413A (en) * | 2021-12-29 | 2022-03-29 | 郑州中科新兴产业技术研究院 | Continuous reaction rectification device and working method thereof |
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| CN103508925A (en) * | 2012-06-29 | 2014-01-15 | 戴东胜 | Preparation method for methanesulfonic acid |
| CN103641748A (en) * | 2013-11-29 | 2014-03-19 | 湖北星火化工有限公司 | Method for preparing methanesulfonic acid by recycling byproduct, namely hydrochloric acid |
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| CN101560173A (en) * | 2008-04-18 | 2009-10-21 | 天津市康沃特科技有限公司 | Synthesis process of electronic-grade high-purity methylsulphonic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114247413A (en) * | 2021-12-29 | 2022-03-29 | 郑州中科新兴产业技术研究院 | Continuous reaction rectification device and working method thereof |
| CN114247413B (en) * | 2021-12-29 | 2024-03-19 | 郑州中科新兴产业技术研究院 | Continuous reaction rectifying device and working method thereof |
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Application publication date: 20170118 |