CN101543745B - Method for preparing dispersant and dispersant - Google Patents
Method for preparing dispersant and dispersant Download PDFInfo
- Publication number
- CN101543745B CN101543745B CN2009100831644A CN200910083164A CN101543745B CN 101543745 B CN101543745 B CN 101543745B CN 2009100831644 A CN2009100831644 A CN 2009100831644A CN 200910083164 A CN200910083164 A CN 200910083164A CN 101543745 B CN101543745 B CN 101543745B
- Authority
- CN
- China
- Prior art keywords
- temperature
- add
- still
- formaldehyde
- insulation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 title abstract 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims abstract description 36
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000007062 hydrolysis Effects 0.000 claims abstract description 22
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000012065 filter cake Substances 0.000 claims abstract description 9
- 238000009833 condensation Methods 0.000 claims abstract description 6
- 230000005494 condensation Effects 0.000 claims abstract description 6
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 96
- 230000003472 neutralizing effect Effects 0.000 claims description 29
- 238000009413 insulation Methods 0.000 claims description 25
- 239000000920 calcium hydroxide Substances 0.000 claims description 23
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 23
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 14
- 238000007664 blowing Methods 0.000 claims description 11
- 238000004458 analytical method Methods 0.000 claims description 10
- 238000006482 condensation reaction Methods 0.000 claims description 10
- 238000010298 pulverizing process Methods 0.000 claims description 10
- 238000005070 sampling Methods 0.000 claims description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 8
- 239000012895 dilution Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000003556 assay Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 235000008733 Citrus aurantifolia Nutrition 0.000 abstract 1
- 235000011941 Tilia x europaea Nutrition 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 239000004571 lime Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract 1
- 239000008267 milk Substances 0.000 abstract 1
- 210000004080 milk Anatomy 0.000 abstract 1
- 235000013336 milk Nutrition 0.000 abstract 1
- 238000009472 formulation Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 239000002994 raw material Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000011265 semifinished product Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000004566 building material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Landscapes
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention provides a method for preparing a dispersant and the dispersant. The dispersant comprises the following formula (by weight ratio): 350 to 480 portions of naphthalene, 450 to 605 portions of sulfuric acid, 155 to 187 portions of formaldehyde, 70 to 100 portions of lime milk 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
Technical field
The present invention relates to a kind of preparation diffusant method and diffusant, belong to the fine chemical technology field.
Background technology
There are the processing technology complexity in existing diffusant and preparation method, defectives such as unstable product quality.
Summary of the invention
In order to overcome the deficiency of prior art structure, the invention provides a kind of preparation diffusant method and diffusant.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of diffusant, prescription (weight proportion) is as follows:
Naphthalene 350-480
Sulfuric acid 450-605
Formaldehyde 155-187
Milk of lime 70-100
Water is an amount of.
A kind of preparation diffusant 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:
Slowly add the formaldehyde according to proportioning quantity in the time of temperature 93-98 ℃, add in the formaldehyde process, temperature must not surpass 95 ℃, closes each Dao Jiemen after formaldehyde adds, and adjusts temperature under 85-95 ℃ of following condition, condensation reaction 2 hours;
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 milk of lime in the measuring tank is slowly added the neutralizing tank reaction;
3, transfer pH value:
After sulfonated bodies has been put, open the reactor manhole cover, rinse remnant in the clean still with running water, rinse still water and put into neutralizing tank, treat that milk of lime quantitatively adds after, will change ready milk of lime in advance and put into neutralizing tank, adjust 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 and can utilize.Beneficial effect: increased output per single reactor, reduced production cost.
Beneficial effect of the present invention also has:
Effect: 1) increased finished product color fastness and stability; 2) raising of temperature has increased the product sufficient reacting in the step 3, has significantly improved finished product output, has reduced production cost.
Effect: 2) liquid caustic soda that will use originally changes into milk of lime.Raw-material adjustment has improved the result of use of product, but also has reduced production cost significantly.
The specific embodiment
Embodiment 1: a kind of preparation diffusant method, contain following steps;
Prepare burden by following prescription (weight proportion):
Naphthalene 350
Sulfuric acid 450
Formaldehyde 155
Milk of lime 70
Water 178 hydrolysis
Before the 131 living temperature
175 dilutions
One, sulfonation
1, dissolving naphthalene:
After checking before feeding intake that production equipment is normal, add the naphthalene of above-mentioned formulation ratio 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:
Slowly add the formaldehyde of above-mentioned formulation ratio when 93 ℃ of temperature, add in the formaldehyde process, temperature must not surpass 95 ℃, close each Dao Jiemen after formaldehyde adds, and adjusts temperature under 85 ℃ of following conditions, condensation reaction 2 hours.
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, the pressure in the water measuring tank must 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, whether clean totally, open the blowing joint door of reactor on the workbench after normal, sulfonated bodies is put into neutralizing tank fast, open neutralizing tank in the time of blowing and stir, the milk of lime in the measuring tank is slowly added the neutralizing tank reaction.
3, transfer pH value:
After sulfonated bodies has been put, open the reactor manhole cover, rinse remnant in the clean still with running water, rinse still water and put into neutralizing tank, treat that milk of lime quantitatively adds after, will change ready milk of lime in advance and put into neutralizing tank, adjust 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/m2.1.00-1.05 is qualified with proportion instrumentation proportion.
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％ |
| Milk of lime | 100 | 81.60 |
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 preparation diffusant method, contain following steps;
Prepare burden by following prescription (weight proportion):
Naphthalene 400
Sulfuric acid 571
Formaldehyde 171
Milk of lime 80
Water 203 hydrolysis
Before the 150 living temperature
200 dilutions
One, sulfonation
1, dissolving naphthalene:
After checking before feeding intake that production equipment is normal, add the naphthalene of above-mentioned formulation ratio 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 95 ℃ of temperature, and temperature must not surpass 95 ℃, close each Dao Jiemen after formaldehyde adds, and adjusts temperature under 89 ℃ of following conditions, condensation reaction 2 hours.
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, the pressure in the water measuring tank must 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, whether clean totally, open the blowing joint door of reactor on the workbench after normal, sulfonated bodies is put into neutralizing tank fast, open neutralizing tank in the time of blowing and stir, the milk of lime in the measuring tank is slowly added the neutralizing tank reaction.
3, transfer pH value:
After sulfonated bodies has been put, open the reactor manhole cover, rinse remnant in the clean still with running water, rinse still water and put into neutralizing tank, treat that milk of lime quantitatively adds after, will change ready milk of lime in advance and put into neutralizing tank, adjust 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/m2.1.00-1.05 is qualified with proportion instrumentation proportion.
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％ |
| Milk of lime | 100 | 81.60 |
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 preparation diffusant method contains following steps;
Prepare burden by following prescription (weight proportion):
Naphthalene 480
Sulfuric acid 605
Formaldehyde 187
Milk of lime 96
Water 243 hydrolysis
Before the 180 living temperature
240 dilutions
One, sulfonation
1, dissolving naphthalene:
After checking before feeding intake that production equipment is normal, add the naphthalene of above-mentioned formulation ratio 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:
Slowly add the formaldehyde of above-mentioned formulation ratio when 98 ℃ of temperature, add in the formaldehyde process, temperature must not surpass 95 ℃, close each Dao Jiemen after formaldehyde adds, and adjusts temperature under 95 ℃ of following conditions, condensation reaction 2 hours.
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, the pressure in the water measuring tank must 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, whether clean totally, open the blowing joint door of reactor on the workbench after normal, sulfonated bodies is put into neutralizing tank fast, open neutralizing tank in the time of blowing and stir, the milk of lime in the measuring tank is slowly added the neutralizing tank reaction.
3, transfer pH value:
After sulfonated bodies has been put, open the reactor manhole cover, rinse remnant in the clean still with running water, rinse still water and put into neutralizing tank, treat that milk of lime quantitatively adds after, will change ready milk of lime in advance and put into neutralizing tank, adjust 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/m2.1.00-1.05 is qualified with proportion instrumentation proportion.
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％ |
| Milk of lime | 100 | 81.60 |
Claims (2)
1. one kind prepares the diffusant method, it 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;
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:
Slowly add the formaldehyde according to proportioning quantity in the time of temperature 93-98 ℃, add in the formaldehyde process, temperature must not surpass 95 ℃, closes each Dao Jiemen after formaldehyde adds, and adjusts temperature under 85-95 ℃ of following condition, condensation reaction 2 hours;
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 milk of lime in the measuring tank is slowly added the neutralizing tank reaction;
3), transfer pH value:
After sulfonated bodies has been put, open the reactor manhole cover, rinse remnant in the clean still with running water, rinse still water and put into neutralizing tank, treat that milk of lime quantitatively adds after, will change ready milk of lime in advance and put into neutralizing tank, adjust 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
Material after filtering is pressed onto in the concentration tank concentrates, 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;
Step 7, drying dry processing with the filter cake after filtering; The feed liquid that collection throws away goes to step 5.
2. a kind of a kind of diffusant for preparing the preparation of diffusant method according to claim 1 is characterized in that weight proportion is as follows:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100831644A CN101543745B (en) | 2009-05-06 | 2009-05-06 | Method for preparing dispersant and dispersant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100831644A CN101543745B (en) | 2009-05-06 | 2009-05-06 | Method for preparing dispersant and dispersant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101543745A CN101543745A (en) | 2009-09-30 |
| CN101543745B true CN101543745B (en) | 2011-09-14 |
Family
ID=41191275
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100831644A Active CN101543745B (en) | 2009-05-06 | 2009-05-06 | Method for preparing dispersant and dispersant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101543745B (en) |
Families Citing this family (2)
| 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 |
| CN106281511A (en) * | 2015-06-08 | 2017-01-04 | 李全灵 | Coal water slurry dispersing agent |
-
2009
- 2009-05-06 CN CN2009100831644A patent/CN101543745B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN101543745A (en) | 2009-09-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100351273C (en) | Heterogeneous carrageenan manufacturing process from mono component seaweed with reduced use of level of koh | |
| CN101786667A (en) | Method for preparing poly-aluminum ferric chloride sulfate and product thereof | |
| CN101891840B (en) | Method for extracting pectin by utilizing potato scraps | |
| CN106629756A (en) | Method for improving oil absorption value by treating white carbon black through alcohols | |
| CN101543745B (en) | Method for preparing dispersant and dispersant | |
| CN101671374B (en) | New technique for extracting D-glucosamine hydrochloride | |
| CN101649336A (en) | Novel process for producing sodium heparin | |
| CN106117072A (en) | A kind of levodopa crystalline powder and manufacture method thereof | |
| CN101543746B (en) | Dispersant and preparation method thereof | |
| CN110407950A (en) | A method of mould intracellular polyse is extracted using green solvent | |
| CN110330213A (en) | A kind of high efficiency composition conditioner for sludge dewatering | |
| CN103804172B (en) | A kind of method improving organic acid production quality | |
| CN102114396A (en) | Non-quinoline dispersant MF and production process | |
| CN107556804B (en) | Production process of high-oil-absorption-value and large-pore-volume flatting agent | |
| CN101632907A (en) | Preparation method of dispersant with high efficiency and low formaldehyde | |
| CN101130797A (en) | Ubelin manufacturing technique | |
| CN107619411A (en) | A kind of ferroheme extracting method | |
| CN110526284A (en) | A kind of preparation method of four basic lead sulphates | |
| CN110372812A (en) | A kind of natural rubber and preparation method thereof with high PO, PRI | |
| CN102060691A (en) | Continuous acidolysis process for calcium hydrogen citrate | |
| CN109136413A (en) | A method of high purity glucose is prepared using cornstarch | |
| CN106538841A (en) | A kind of dried porcine saluble product and its production method | |
| CN109090336A (en) | A kind of rice protein powder extracting method increasing protein content | |
| CN109355949A (en) | A kind of without phosphorus liquid substitute alkali and preparation method thereof | |
| CN102125162B (en) | Method for processing citric-acid fermented liquor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Owner name: LI XIUYUN Free format text: FORMER OWNER: BEIJING HUAZHONG NEW INDUSTRY + TRADE CO., LTD. Effective date: 20100812 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 101407 YANXI INDUSTRY DEVELOPMENT ZONE, HUAIROU DISTRICT, BEIJING CITY TO: 101407 NO.30, YANXIDONGER ROAD, YANXI ECONOMIC DEVELOPMENT ZONE, HUAIROU DISTRICT, BEIJING CITY |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20100812 Address after: 101407 Beijing city Huairou District Yanqi Yanqi Economic Development Zone, two East Road No. 30 Applicant after: Li Xiuyun Address before: 101407 Beijing Huairou Yanqi Industrial Development Zone Applicant before: Beijing Huazhong New Industry & Trade Co., Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190409 Address after: 063300 Lingang Economic Development Zone, Fengnan District, Tangshan City, Hebei Province Patentee after: Huazhong Xinsheng (Tangshan) Fluorescent Materials Co., Ltd. Address before: 101407 No. 30 Yanqi East Second Road, Yanqi Economic Development Zone, Huairou District, Beijing Patentee before: Li Xiuyun |
|
| TR01 | Transfer of patent right |