CN101543746B - Dispersant and preparation method thereof - Google Patents

Dispersant and preparation method thereof Download PDF

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Publication number
CN101543746B
CN101543746B CN2009100831659A CN200910083165A CN101543746B CN 101543746 B CN101543746 B CN 101543746B CN 2009100831659 A CN2009100831659 A CN 2009100831659A CN 200910083165 A CN200910083165 A CN 200910083165A CN 101543746 B CN101543746 B CN 101543746B
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temperature
add
still
formaldehyde
insulation
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CN101543746A (en
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李秀云
张仲元
万建莲
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Huazhong Xinsheng (Tangshan) Fluorescent Materials Co., Ltd.
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Beijing Huazhong New Industry & Trade Co Ltd
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Abstract

The invention provides a dispersant and a preparation method thereof. The dispersant comprises: 350 to 480 portions of naphthalene, 450 to 605 portions of sulfuric acid, 155 to 187 portions of formaldehyde, 285.5 to 343 portions of liquid caustic soda and proper amount of water. The method for preparing the dispersant comprises the steps of sulfonation, hydrolysis, condensation, neutralization, concentration, drying and grinding. The processing process is simple, the product has stable quality, a spin-dry procedure (a filter cake is directly poured out in the prior process) is added, a drier device is added to perform spin-dry processing on the prior directly poured filter cake, and the poured feed liquor is collected and used in the way. The preparation method increases the single-autoclave output and reduces the production cost.

Description

A kind of diffusant and preparation method
Technical field
The present invention relates to a kind of diffusant and preparation method, belong to the fine chemical technology field.
Background technology
Existing diffusant and preparation method exist processing technology complicated, defectives such as unstable product quality.
Summary of the invention
In order to overcome the deficiency of prior art structure, the present invention provides a kind of diffusant and preparation method.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of diffusant, fill a prescription (weight proportion) as follows:
Naphthalene 350-480
Sulfuric acid 450-605
Formaldehyde 155-187
Liquid caustic soda 285.5-343
Water is an amount of.
A kind of diffusant preparation method contains following steps;
Step 1, sulfonation
1, dissolving naphthalene:
Select refined naphthalene according to proportioning quantity, add at twice in the still, add steam in the still, give birth to temperature, pressurization is opened to stir and is continued to heat up;
2, add acid:
When temperature rises to 105 ℃, will once add in the still according to the sulfuric acid of proportioning quantity, add and close the joint door, continue to be warming up between 110-125 ℃;
3, insulation: keep under 120 ℃ of conditions in temperature, continue to stir 0.5 hour;
Step 2, hydrolysis
1, sample analysis total acidity: open stirring after the sampling;
2, cooling: after total acidity is qualified, close jacket steam, temperature in the kettle is descended about 10 minutes naturally, chuck leads to running water, and temperature is reduced to 80 ℃ of hydrolysis to be added;
3, Jia Shui: in temperature during, in quantitative running water added jar, finish and stirred hydrolysis 60 minutes at 80 ℃;
Step 3, condensation
1, add formaldehyde:
When 80 ℃ of temperature, slowly add the formaldehyde according to proportioning quantity, add in the formaldehyde process, temperature must not surpass 85 ℃, close each Dao Jiemen after formaldehyde adds, the adjustment temperature under 85 ℃ of following conditions, condensation reaction 1 hour;
2, insulation: formaldehyde finishes turns off the joint door, and condensation reaction is 2 hours under 80 ℃ of conditions of adjustment temperature;
3, heat up: after insulation finishes, add the logical jacket steam of quantitative running water and heat up, the variation of pressure is observed in the cock of opening still upward pressure table simultaneously, and insulation is 2 hours when temperature reaches 90 ℃, this moment the still internal pressure at 0.01Mpa, about;
Step 4, neutralization
1, dilution:
Insulation once is pressed into quantitative water in the still with compressed air after finishing,
2 neutralizations:
Sulfonated bodies is put into neutralizing tank, open neutralizing tank in the time of blowing and stir, the liquid caustic soda in the measuring tank is slowly added the neutralizing tank reaction;
3, transfer pH value:
After sulfonated bodies has been put, open the agitated reactor manhole cover, rinse the remnant in the clean still with running water; Rinse still water and put into neutralizing tank, treat that liquid caustic soda quantitatively adds after, will change ready liquid caustic soda in advance and put into neutralizing tank; Adjustment pH value 9-10; Volume is transferred in qualified back, the content and the pH value of lab technician's sample analysis sodium sulphate, qualified back discharging to be filtered;
Step 5, concentrated
Being pressed onto in the concentration tank after filtering concentrated, and concentration tank leads to jacket steam, and pressure is no more than 2kg/m2; With proportion instrumentation proportion;
Step 6, drying, pulverizing
1, the material that drying is concentrated is put into the drum groove, starts drum and dries, and drum pressure requires to be no more than 3kg/m2, and the lab technician analyzes content, the PH of sodium sulphate;
2, after the assay was approved, dried material is put into pulverizer pulverize, pulverizing finishes, and lab technician's sampling is tested;
Beneficial effect of the present invention, processing technology is simple, and constant product quality is widely used in building materials, weaving, plating and rubber industry.Application market has a extensive future, and can form good economic benefit and social benefit.
Newly-increased filter cake dries program (former technology filter cake is directly outwelled) on original basis.Newly-increased drier equipment dries processing with the former filter cake of directly outwelling, and the feed liquid that throws away like this collects capable of using.Beneficial effect: increased output per single reactor, reduced production cost.
The specific embodiment
Embodiment 1: a kind of diffusant preparation method, contain following steps;
Prepare burden by following prescription (weight proportion):
Naphthalene 350
Sulfuric acid 450
Formaldehyde 155
Liquid caustic soda 249 (to roll over hundred cubage throwing amounts)
Water 178 hydrolysis
Before the 131 living temperature
175 dilutions
One, sulfonation
1, dissolving naphthalene:
Before feeding intake the inspection production equipment normal after, the naphthalene of above-mentioned formulation ratio is added in the still at twice, build port lid then; First-class manhole clamp; Logical jacket steam is given birth to temperature, and steam pressure remains between the 2-3kg/m2; The highest 3kg/m2 that must not surpass treats that temperature in the kettle rises to 100 ℃, opens to stir and continues to give birth to temperature.
2, add acid:
When temperature rises to 105 ℃, the sulfuric acid of above-mentioned formulation ratio is once added in the still, add and close the joint door, continue to be warming up between 110-125 ℃.
3, insulation: keep under 120 ℃ of conditions in temperature, continue to stir 0.5 hour.
Two, hydrolysis
1, sample analysis total acidity:
After sulfonating reaction finishes, at first close stirring, open sample tap, take a sample with carrying spoon, analyzing total acidity, requiring is qualified between 18.5-23.If acidity is too high, can prolong temperature retention time or when hydrolysis, add a little water in right amount, in time open stirring after the sampling.
2, cooling:
After total acidity is qualified, close jacket steam, temperature in the kettle is descended about 10 minutes naturally, chuck leads to running water, and temperature is reduced to 80 ℃ of hydrolysis to be added.
3, Jia Shui:
In temperature during, in quantitative running water added jar, finish and stirred hydrolysis 60 minutes at 80 ℃.
Three, condensation
1, add formaldehyde:
When 80 ℃ of temperature, slowly add the formaldehyde of above-mentioned formulation ratio, add in the formaldehyde process, temperature must not surpass 85 ℃, close each Dao Jiemen after formaldehyde adds, the adjustment temperature under 85 ℃ of following conditions, condensation reaction 1 hour.
2, insulation: formaldehyde finishes turns off the joint door, and condensation reaction is 2 hours under 80 ℃ of conditions of adjustment temperature.
3, heat up: after insulation finishes, add the logical jacket steam of quantitative running water and heat up, the variation of pressure is observed in the cock of opening still upward pressure table simultaneously, and insulation is 2 hours when temperature reaches 90 ℃, this moment the still internal pressure at 0.01Mpa, about.
Four, neutralization
1, dilution:
After insulation finishes, quantitative water once is pressed in the still, must the pressure in the water measuring tank be raised to when noting adding water could open and adds water and save, otherwise flow backwards, cause the accident greater than the still internal pressure with compressed air.
2 neutralizations:
Whether will check in advance before the blowing does not have material in the neutralizing tank; Clean whether is opened the blowing joint door of agitated reactor on the workbench after normal, and sulfonated bodies is put into neutralizing tank fast; Open neutralizing tank in the time of blowing and stir, the liquid caustic soda in the measuring tank is slowly added the neutralizing tank reaction.
3, transfer pH value:
After sulfonated bodies has been put, open the agitated reactor manhole cover, rinse the remnant in the clean still with running water; Rinse still water and put into neutralizing tank, treat that liquid caustic soda quantitatively adds after, will change ready liquid caustic soda in advance and put into neutralizing tank; Adjustment pH value 9-10; Volume is transferred in qualified back, the content and the pH value of lab technician's sample analysis sodium sulphate, qualified back discharging to be filtered.
Five, concentrate
Being pressed onto in the concentration tank after filtering concentrated, and concentration tank leads to jacket steam, and pressure is no more than 2kg/m2.It is qualified using proportion instrumentation proportion 1.00-1.05.
Six, dry, pulverizing
1, the material that drying is concentrated is put into the drum groove, starts drum and dries, and drum pressure requires to be no more than 3kg/m2, and the lab technician analyzes content, the PH of sodium sulphate.
2, after the assay was approved, dried material is put into pulverizer pulverize, pulverizing finishes, and lab technician's sampling is tested by " company's raw material semi-finished product, product inspection plan ".
Diffusion agent N NZ prescription
The raw material title Molecular weight Pure quality Content
Naphthalene 128 408 100%
Sulfuric acid 98 560 98%
Formaldehyde 30 63.3 37%
Liquid caustic soda 40.01 285.5 32%
Step 7, drying
Filter cake after filtering is dried processing; The feed liquid that collection throws away goes to step 5.
Embodiment 2: a kind of diffusant preparation method, contain following steps;
Prepare burden by following prescription (weight proportion):
Naphthalene 400
Sulfuric acid 571
Formaldehyde 171
Liquid caustic soda 285.5 (to roll over hundred cubage throwing amounts)
Water 203 hydrolysis
Before the 150 living temperature
200 dilutions
One, sulfonation
1, dissolving naphthalene:
Before feeding intake the inspection production equipment normal after, the naphthalene of above-mentioned formulation ratio is added in the still at twice, build port lid then; First-class manhole clamp; Logical jacket steam is given birth to temperature, and steam pressure remains between the 2-3kg/m2; The highest 3kg/m2 that must not surpass treats that temperature in the kettle rises to 100 ℃, opens to stir and continues to give birth to temperature.
2, add acid:
When temperature rises to 105 ℃, the sulfuric acid of above-mentioned formulation ratio is once added in the still, add and close the joint door, continue to be warming up between 110-125 ℃.
3, insulation: keep under 120 ℃ of conditions in temperature, continue to stir 0.5 hour.
Two, hydrolysis
1, sample analysis total acidity:
After sulfonating reaction finishes, at first close stirring, open sample tap, take a sample with carrying spoon, analyzing total acidity, requiring is qualified between 18.5-23.If acidity is too high, can prolong temperature retention time or when hydrolysis, add a little water in right amount, in time open stirring after the sampling.
2, cooling:
After total acidity is qualified, close jacket steam, temperature in the kettle is descended about 10 minutes naturally, chuck leads to running water, and temperature is reduced to 80 ℃ of hydrolysis to be added.
3, Jia Shui:
In temperature during, in quantitative running water added jar, finish and stirred hydrolysis 60 minutes at 80 ℃.
Three, condensation
1, add formaldehyde:
The formaldehyde of slow above-mentioned formulation ratio adds in the formaldehyde process when 80 ℃ of temperature, and temperature must not surpass 85 ℃, close each Dao Jiemen after formaldehyde adds, the adjustment temperature under 85 ℃ of following conditions, condensation reaction 1 hour.
2, insulation: formaldehyde finishes turns off the joint door, and condensation reaction is 2 hours under 80 ℃ of conditions of adjustment temperature.
3, heat up: after insulation finishes, add the logical jacket steam of quantitative running water and heat up, the variation of pressure is observed in the cock of opening still upward pressure table simultaneously, and insulation is 2 hours when temperature reaches 90 ℃, this moment the still internal pressure at 0.01Mpa, about.
Four, neutralization
1, dilution:
After insulation finishes, quantitative water once is pressed in the still, must the pressure in the water measuring tank be raised to when noting adding water could open and adds water and save, otherwise flow backwards, cause the accident greater than the still internal pressure with compressed air.
2 neutralizations:
Whether will check in advance before the blowing does not have material in the neutralizing tank; Clean whether is opened the blowing joint door of agitated reactor on the workbench after normal, and sulfonated bodies is put into neutralizing tank fast; Open neutralizing tank in the time of blowing and stir, the liquid caustic soda in the measuring tank is slowly added the neutralizing tank reaction.
3, transfer pH value:
After sulfonated bodies has been put, open the agitated reactor manhole cover, rinse the remnant in the clean still with running water; Rinse still water and put into neutralizing tank, treat that liquid caustic soda quantitatively adds after, will change ready liquid caustic soda in advance and put into neutralizing tank; Adjustment pH value 9-10; Volume is transferred in qualified back, the content and the pH value of lab technician's sample analysis sodium sulphate, qualified back discharging to be filtered.
Five, concentrate
Being pressed onto in the concentration tank after filtering concentrated, and concentration tank leads to jacket steam, and pressure is no more than 2kg/m2.It is qualified using proportion instrumentation proportion 1.00-1.05.
Six, dry, pulverizing
1, the material that drying is concentrated is put into the drum groove, starts drum and dries, and drum pressure requires to be no more than 3kg/m2, and the lab technician analyzes content, the PH of sodium sulphate.
2, after the assay was approved, dried material is put into pulverizer pulverize, pulverizing finishes, and lab technician's sampling is tested by " company's raw material semi-finished product, product inspection plan ".
Diffusion agent N NZ prescription
The raw material title Molecular weight Pure quality Content
Naphthalene 128 408 100%
Sulfuric acid 98 560 98%
Formaldehyde 30 63.3 37%
Liquid caustic soda 40.01 285.5 32%
Step 7, drying
Filter cake after filtering is dried processing; The feed liquid that collection throws away goes to step 5.
Embodiment 3:
A kind of diffusant preparation method contains following steps;
Prepare burden by following prescription (weight proportion):
Naphthalene 480
Sulfuric acid 605
Formaldehyde 187
Liquid caustic soda 343 (to roll over hundred cubage throwing amounts)
Water 243 hydrolysis
Before the 180 living temperature
240 dilutions
One, sulfonation
1, dissolving naphthalene:
Before feeding intake the inspection production equipment normal after, the naphthalene of above-mentioned formulation ratio is added in the still at twice, build port lid then; First-class manhole clamp; Logical jacket steam is given birth to temperature, and steam pressure remains between the 2-3kg/m2; The highest 3kg/m2 that must not surpass treats that temperature in the kettle rises to 100 ℃, opens to stir and continues to give birth to temperature.
2, add acid:
When temperature rises to 105 ℃, the sulfuric acid of above-mentioned formulation ratio is once added in the still, add and close the joint door, continue to be warming up between 110-125 ℃.
3, insulation: keep under 120 ℃ of conditions in temperature, continue to stir 0.5 hour.
Two, hydrolysis
1, sample analysis total acidity:
After sulfonating reaction finishes, at first close stirring, open sample tap, take a sample with carrying spoon, analyzing total acidity, requiring is qualified between 18.5-23.If acidity is too high, can prolong temperature retention time or when hydrolysis, add a little water in right amount, in time open stirring after the sampling.
2, cooling:
After total acidity is qualified, close jacket steam, temperature in the kettle is descended about 10 minutes naturally, chuck leads to running water, and temperature is reduced to 80 ℃ of hydrolysis to be added.
3, Jia Shui:
In temperature during, in quantitative running water added jar, finish and stirred hydrolysis 60 minutes at 80 ℃.
Three, condensation
1, add formaldehyde:
When 80 ℃ of temperature, slowly add the formaldehyde of above-mentioned formulation ratio, add in the formaldehyde process, temperature must not surpass 85 ℃, close each Dao Jiemen after formaldehyde adds, the adjustment temperature under 85 ℃ of following conditions, condensation reaction 1 hour.
2, insulation: formaldehyde finishes turns off the joint door, and condensation reaction is 2 hours under 80 ℃ of conditions of adjustment temperature.
3, heat up: after insulation finishes, add the logical jacket steam of quantitative running water and heat up, the variation of pressure is observed in the cock of opening still upward pressure table simultaneously, and insulation is 2 hours when temperature reaches 90 ℃, this moment the still internal pressure at 0.01Mpa, about.
Four, neutralization
1, dilution:
After insulation finishes, quantitative water once is pressed in the still, must the pressure in the water measuring tank be raised to when noting adding water could open and adds water and save, otherwise flow backwards, cause the accident greater than the still internal pressure with compressed air.
2 neutralizations:
Whether will check in advance before the blowing does not have material in the neutralizing tank; Clean whether is opened the blowing joint door of agitated reactor on the workbench after normal, and sulfonated bodies is put into neutralizing tank fast; Open neutralizing tank in the time of blowing and stir, the liquid caustic soda in the measuring tank is slowly added the neutralizing tank reaction.
3, transfer pH value:
After sulfonated bodies has been put, open the agitated reactor manhole cover, rinse the remnant in the clean still with running water; Rinse still water and put into neutralizing tank, treat that liquid caustic soda quantitatively adds after, will change ready liquid caustic soda in advance and put into neutralizing tank; Adjustment pH value 9-10; Volume is transferred in qualified back, the content and the pH value of lab technician's sample analysis sodium sulphate, qualified back discharging to be filtered.
Five, concentrate
Being pressed onto in the concentration tank after filtering concentrated, and concentration tank leads to jacket steam, and pressure is no more than 2kg/m2.It is qualified using proportion instrumentation proportion 1.00-1.05.
Six, dry, pulverizing
1, the material that drying is concentrated is put into the drum groove, starts drum and dries, and drum pressure requires to be no more than 3kg/m2, and the lab technician analyzes content, the PH of sodium sulphate.
2, after the assay was approved, dried material is put into pulverizer pulverize, pulverizing finishes, and lab technician's sampling is tested by " company's raw material semi-finished product, product inspection plan ".
Step 7, drying
Filter cake after filtering is dried processing; The feed liquid that collection throws away goes to step 5.
Diffusion agent N NZ uses equipment
Enamel still 2000L; Neutralizing tank 5000L; 2 of storage tanks; 2 in filter basin; 3 of evaporators; 2 on cylinder; 2 in vavuum pump; 1 on compressor.
Diffusion agent N NZ prescription
The raw material title Molecular weight Pure quality Content
Naphthalene 128 408 100%
Sulfuric acid 98 560 98%
Formaldehyde 30 63.3 37%
Liquid caustic soda 40.01 285.5 32%

Claims (2)

1. a diffusant preparation method is characterized in that containing following steps;
Step 1, sulfonation
1), dissolving naphthalene:
Select refined naphthalene according to proportioning quantity, add at twice in the still, add steam in the still, heat up, pressurization is opened to stir and is continued to heat up;
Weight proportion is following:
Figure FSB00000706728700011
2), add acid:
When temperature rises to 105 ℃, will once add in the still according to the sulfuric acid of proportioning quantity, add and close the joint door, continue to be warming up between 110-125 ℃;
3), insulation: keep under 120 ℃ of conditions in temperature, continue to stir 0.5 hour;
Step 2, hydrolysis
1), sample analysis total acidity: open stirring after the sampling;
2), cooling: after total acidity is qualified, close jacket steam, temperature in the kettle was descended 10 minutes naturally, chuck leads to running water, and temperature is reduced to 80 ℃ of hydrolysis to be added;
3), add water: in temperature during, in quantitative running water added jar, finish and stirred hydrolysis 60 minutes at 80 ℃;
Step 3, condensation
1), add formaldehyde:
When 80 ℃ of temperature, slowly add the formaldehyde according to proportioning quantity, add in the formaldehyde process, temperature must not surpass 85 ℃, close each Dao Jiemen after formaldehyde adds, the adjustment temperature under 85 ℃ of following conditions, condensation reaction 1 hour;
2), insulation: formaldehyde finishes turns off the joint door, and condensation reaction is 2 hours under 80 ℃ of conditions of adjustment temperature;
3), heat up: after insulation finishes, add the logical jacket steam of quantitative running water and heat up, the variation of pressure is observed in the cock of opening still upward pressure table simultaneously, and insulation is 2 hours when temperature reaches 90 ℃, and this moment, the still internal pressure was at 0.01Mpa;
Step 4, neutralization
1), dilution:
Insulation once is pressed into quantitative water in the still with compressed air after finishing,
2), neutralization:
Sulfonated bodies is put into neutralizing tank, open neutralizing tank in the time of blowing and stir, the liquid caustic soda in the measuring tank is slowly added the neutralizing tank reaction;
3), transfer pH value:
After sulfonated bodies has been put, open the agitated reactor manhole cover, rinse the remnant in the clean still with running water; Rinse still water and put into neutralizing tank, treat that liquid caustic soda quantitatively adds after, will change ready liquid caustic soda in advance and put into neutralizing tank; Adjustment pH value 9-10; Volume is transferred in qualified back, the content and the pH value of lab technician's sample analysis sodium sulphate, qualified back discharging to be filtered;
Step 5, concentrated
Leaching after the discharging filtration to be filtered of step 4 expected to be pressed onto in the concentration tank to concentrate, and concentration tank leads to jacket steam, and pressure is no more than 2kg/ square metre; With proportion instrumentation proportion;
Step 6, drying, pulverizing
1), material that drying is concentrated puts into the drum groove, starts drum and dries, drum pressure requires to be no more than 3kg/ square metre, the lab technician analyzes content, the PH of sodium sulphate;
2), after the assay was approved, dried material is put into pulverizer pulverize, pulverizing finishes, and lab technician's sampling is tested.
2. a kind of diffusant preparation method according to claim 1 is characterized in that containing step 7, drying, and the filter cake after filtering is dried processing; The feed liquid that collection throws away goes to step 5.
CN2009100831659A 2009-05-06 2009-05-06 Dispersant and preparation method thereof Active CN101543746B (en)

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102114396A (en) * 2010-12-10 2011-07-06 江阴市盛通化工有限公司 Non-quinoline dispersant MF and production process
CN103613519A (en) * 2013-12-06 2014-03-05 安阳市双环助剂有限责任公司 Production method for dispersing agent XY

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1109092A (en) * 1994-03-22 1995-09-27 天津石油化工公司职工大学 Treatment of sulfuric acid dregs and dye dispersing agent prepared from it
CN1814565A (en) * 2005-01-31 2006-08-09 花王株式会社 Process for producing a naphthalenesulfonate formaldehyde condensate
CN101376639A (en) * 2008-09-28 2009-03-04 浙江闰土股份有限公司 Method for producing dispersant MF and co-producing sodium sulfite

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1109092A (en) * 1994-03-22 1995-09-27 天津石油化工公司职工大学 Treatment of sulfuric acid dregs and dye dispersing agent prepared from it
CN1814565A (en) * 2005-01-31 2006-08-09 花王株式会社 Process for producing a naphthalenesulfonate formaldehyde condensate
CN101376639A (en) * 2008-09-28 2009-03-04 浙江闰土股份有限公司 Method for producing dispersant MF and co-producing sodium sulfite

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