CN110368715A - The impurity minimizing technology and device of Sulfonates anionic surfactant - Google Patents
The impurity minimizing technology and device of Sulfonates anionic surfactant Download PDFInfo
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- CN110368715A CN110368715A CN201810324774.8A CN201810324774A CN110368715A CN 110368715 A CN110368715 A CN 110368715A CN 201810324774 A CN201810324774 A CN 201810324774A CN 110368715 A CN110368715 A CN 110368715A
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- poromerics
- anionic surfactant
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/206—Packing or coating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
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Abstract
The invention discloses a kind of impurity minimizing technologies of Sulfonates anionic surfactant.This method is used to carry out poromerics adsorption treatment to the acidic sulfonated object handled by process for sulfonation, to remove sulfur trioxide in product and sulfuric acid and unsulfonated material；Wherein, the poromerics includes the second poromerics of the first poromerics and aperture greater than 0.45nm that aperture is 0.40-0.45nm.The first poromerics load has cobalt chloride crystal or copper sulfate crystal or nickel sulfate hexahydrate crystal.The invention also discloses the devices for realizing this method.The present invention can effectively remove the inorganic acid or inorganic salts of 30-70% in the sulfonated products of Sulfonates anionic surfactant, can more remove the unsulfonated material of 20-60%, improve the gross activity object content of product.The present invention is not for influencing its production capacity, and equipment investment expense and lower production costs in the production technology of Sulfonates anionic surfactant.
Description
Technical field
The present invention relates to a kind of impurity minimizing technology of Sulfonates anionic surfactant and devices.
Background technique
Currently, Sulfonates anionic surfactant uses process for sulfonation in its preparation process and remains in the product
There are inorganic acid or inorganic salts (predominantly sulfuric acid or sulfate) and unsulfonated material (such as alkene and alkane, alkylbenzene and aliphatic ester)
Equal impurity.Moreover, because the product mineral acid content after process for sulfonation is higher, alkali required for subsequent neutralization procedure is caused to be used
Amount increases, and also makes the active matter content of finished product relatively low.
Summary of the invention
The first purpose of this invention is to provide a kind of impurity minimizing technology of Sulfonates anionic surfactant,
Effectively to solve the deficiencies in the prior art place.
Second object of the present invention is to provide a kind of device for realizing the above method.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
The impurity minimizing technology of Sulfonates anionic surfactant, to the acid sulphur handled by process for sulfonation
Compound carries out poromerics adsorption treatment, to remove sulfur trioxide in product and sulfuric acid and unsulfonated material；Wherein, described
Poromerics includes the second poromerics that the first poromerics that aperture is 0.40-0.45nm and aperture are greater than 0.45nm.
Preferably, first poromerics and the second poromerics are inorganic microporous material, including micropore sial
Hydrochlorate, mesoporous silica, micropore borophosphate, aluminium phosphate molecular sieve and micropore ceramics.
Preferably, the first poromerics load has cobalt chloride crystal or copper sulfate crystal or nickel sulfate hexahydrate crystal.
Preferably, being carried out after the crystallization water that the first poromerics is loaded is totally consumed to the first poromerics
It lives again processing, the processing of living again includes adsorbate desorption and crystallization water generation step.
As a kind of selection, the aperture of second poromerics is greater than 0.45 and is less than or equal to 0.50nm, to remove
Alkene and alkane in product；The ratio of first poromerics and the second poromerics is 1:0.8~1:2；It is described two
Poromerics is arranged using hybrid mode or subsection setup.
Alternatively, the aperture of second poromerics is 0.70-0.80nm, to remove the alkane in product
Base benzene and aliphatic ester；The ratio of first poromerics and the second poromerics is 1:0.8~1:2；Described two micropores
Material is arranged using hybrid mode or subsection setup.
To reach second purpose, the present invention adopts the following technical scheme:
The impurity removal means of Sulfonates anionic surfactant, be arranged in process for sulfonation equipment discharging pipeline and
Between finished cylinder, comprising: absorption pipeline is arranged in parallel by least one adsorption tube, and total caliber of the absorption pipeline is sulfonation
2~3 times of the discharging pipeline caliber of process equipment；And poromerics, it is filled in the absorption pipeline, loading is 0.2~1
Cubic meter.
Preferably, the poromerics includes that the first poromerics that aperture is 0.40-0.45nm and aperture are greater than
The second poromerics of 0.45nm；First poromerics and the second poromerics are inorganic microporous material, including micropore
Alumino-silicate, mesoporous silica, micropore borophosphate, aluminium phosphate molecular sieve and micropore ceramics；First poromerics is negative
It is loaded with cobalt chloride crystal or copper sulfate crystal or nickel sulfate hexahydrate crystal.
Preferably, the ratio of first poromerics and second poromerics is 1:0.8~1:2；Described
One poromerics and the first poromerics are using hybrid mode filling or subsection filling.
Preferably, the aperture of second poromerics is greater than 0.45 and to be less than or equal to 0.50nm；Or described second
The aperture of poromerics is 0.70-0.80nm.
The present invention can effectively remove in the sulfonated products of Sulfonates anionic surfactant the inorganic acid of 30-70% or
Inorganic salts can more remove the unsulfonated material of 20-60%, improve the gross activity object content of product.The present invention is used for Sulfonates
In the production technology of anionic surfactant, its production capacity, and equipment investment expense and lower production costs are not influenced.
Detailed description of the invention
Fig. 1 is the structure principle chart of the impurity removal means of Sulfonates anionic surfactant of the present invention.
In figure:
1-adsorption tube；11-feed inlets；12-discharge ports；2-the first poromerics；3-the second poromerics.
Now in conjunction with drawings and examples, invention is further described in detail.
Specific embodiment
As shown in Figure 1, the impurity removal means of Sulfonates anionic surfactant of the present invention, have one
Pipeline is adsorbed, which routes at least one adsorption tube 1 (the present embodiment is one) and be arranged in parallel, and adsorbs the feed inlet of pipeline
11 then connect with finished cylinder with the discharging piping connection of process for sulfonation equipment, discharge port 12；Total caliber of absorption pipeline should be
2~3 times of the discharging pipeline caliber of process for sulfonation equipment.0.2~1 cubic metre of poromerics is also filled in absorption pipeline.
Poromerics using inorganic microporous material (including micropore alumino-silicate, mesoporous silica, micropore borophosphate,
Aluminium phosphate molecular sieve and micropore ceramics).Poromerics is divided into the first poromerics 2 and the second poromerics 3, and subsection filling is being inhaled
In attached pipe 1；The filling proportion of first poromerics and the second poromerics is 1:0.8~1:2.Wherein, first poromerics 2
Aperture is 0.40-0.45nm, and load has cobalt chloride crystal or copper sulfate crystal or nickel sulfate hexahydrate crystal, in adsorbed product
Sulfur trioxide and sulfuric acid.Second poromerics 2 uses aperture for the poromerics greater than 0.45 and less than or equal to 0.50nm, uses
To remove the alkene and alkane in product；Or second poromerics 2 use aperture for the poromerics of 0.70-0.80nm, to
Remove the alkylbenzene and aliphatic ester in product.
It should be noted that the first poromerics and the second poromerics also may be mixed together filling.
In addition, working as above-mentioned poromerics after a period of use, poromerics adsorbate saturation is needed at this time to poromerics
Processing of living again is carried out, concrete mode is as follows:
1, the processing of living again of the first poromerics:
The cobalt chloride crystal or copper sulfate crystal or nickel sulfate hexahydrate crystal of first poromerics 2 load, except being used for and product
In sulfur trioxide water reaction occur generate outside sulfuric acid, also with the characteristic of indicator, i.e. cobalt chloride crystal is designated as red, sulphur
Sour copper crystal is designated as blue, nickel sulfate hexahydrate crystal is designated as blue.After the crystallization water completely consumes, then cobalt chloride is designated as indigo plant
Color, copper sulphate are designated as white, nickel sulfate is designated as yellow green, then need to carry out processing of living again to the first poromerics.First is micro-
The Porous materials processing step that live again is as follows: firstly, the first poromerics is taken out and is soaked in deionized water, in stirring
It is slowly added to sodium hydroxide solution under state, until the pH of solution is 7.0~7.5, the H in micropore2SO4Complete neutralization obtains sulfuric acid
Sodium, and be desorbed in micropore；Then, the moisture for leaching the first poromerics surface, the first poromerics is dried in vacuo, and is steamed
Send out moisture in micropore；Finally, carrying out constant temperature and humidity processing under conditions of 35~40 DEG C, humidity are 80%~90%, make first
Poromerics shows the color of loaded crystalline hydrate, and color is uniform.
2, the processing of living again of the second poromerics:
Firstly, organic solvent (such as alcohol, ether, ketone, esters after the second poromerics is taken out with total carbon number less than or equal to 4
Solvent, such as ethyl alcohol, acetone, ether, ethyl acetate) the second poromerics is impregnated, make unsulfonated monomer desorption in the second micropore
Material；Finally, leaching the solvent of the second poromerics, and the second poromerics is evaporated under reduced pressure, is evaporated molten in micropore
Agent.
3, the mixing of the first poromerics and the second poromerics is lived again processing；
Firstly, being soaked in deionization after poromerics (the first poromerics and the second poromerics mix filling) is taken out
In water, it is slowly added to sodium hydroxide solution while stirring, until the pH of solution is 7.0~7.5, the H in micropore2SO4Completely
It neutralizes, obtains sodium sulphate, and be desorbed in micropore；Then, the moisture on poromerics surface is leached；Then, with total carbon number be less than etc.
Organic solvent (such as alcohol, ether, ketone, esters solvent, such as ethyl alcohol, acetone, ether, ethyl acetate) in 4 impregnates poromerics, makes
Unsulfonated monomer is desorbed in poromerics；Followed by, poromerics is dried in vacuo, evaporate micropore in solvent and water；
Finally, 35~40 DEG C, humidity be 80%~90% under conditions of carry out constant temperature and humidity processing, make first in poromerics micro-
Porous materials show the color of loaded crystalline hydrate, and color is uniform.
Illustrate the present invention below to remove the impurity in four kinds of main Sulfonates anionic surfactants.
Embodiment 1
Alkyl benzene sulfonate anionic surfactant:
Produce the sulfonation equipment of the surfactant production capacity be 3 tons/when, adsorb pipeline total caliber be sulfonation equipment
2 times of discharge nozzle caliber.The loading of poromerics is 0.5 cubic metre, wherein the loading of the first poromerics is 0.2 cube
Rice, the loading of the second poromerics are 0.3 cubic metre, the two subsection filling.The aperture of second poromerics is 0.70-
0.75nm.Impurity removal effect see the table below:
| Before absorption | After absorption | |
| Gross activity object content/% | 96.3 | 97.8 |
| Inorganic acid/% | 1.48 | 0.5 |
| Free oil/% | 1.8 | 0.9 |
| Color/Klett | 48 | 28 |
Embodiment 2
Alpha-alkene sulfonate analog anion surfactants:
Produce the surfactant sulfonation equipment production capacity be 5 tons/when, adsorb total caliber of pipeline be sulfonation equipment discharge
3 times of pipe caliber.Poromerics loading is 1m3, wherein the loading of the first poromerics is 0.45m3, the second poromerics
Loading be 0.55m3, the two subsection filling.The aperture of second poromerics is greater than 0.45 and to be less than or equal to 0.50nm.It is miscellaneous
Matter removal effect see the table below:
Embodiment 3
Fatty acid methyl ester sulfonate anionic surfactant:
Produce the surfactant sulfonation equipment production capacity be 1 ton/when, adsorb total caliber of pipeline be sulfonation equipment discharge
2.5 times of pipe caliber.Poromerics loading is 0.2m3, wherein the loading of the first poromerics is 0.1m3, the second micropore material
The loading of material is 0.1m3, the two subsection filling.The aperture of second poromerics is 0.75~0.80nm.Impurity removal effect
It see the table below:
Embodiment 4
Alkane sulfonic acid salt anionic surfactant:
Produce the surfactant sulfonation equipment production capacity be 3 tons/when, adsorb total caliber of pipeline be sulfonation equipment discharge
2.5 times of pipe caliber.Poromerics loading is 0.8m3, wherein the loading of the first poromerics is 0.27m3, the second micropore
The loading of material is 0.53m3, the two subsection filling.The aperture of second poromerics is greater than 0.45 and to be less than or equal to
0.50nm.Impurity removal effect see the table below:
Claims (10)
1. the impurity minimizing technology of Sulfonates anionic surfactant, which is characterized in that handle by process for sulfonation
The acidic sulfonated object that arrives carries out poromerics adsorption treatment, to remove sulfur trioxide in product and sulfuric acid and unsulfonated material；
Wherein, the poromerics includes that the first poromerics that aperture is 0.40-0.45nm and aperture are second micro- greater than 0.45nm
Porous materials.
2. the impurity minimizing technology of Sulfonates anionic surfactant according to claim 1, which is characterized in that institute
It states the first poromerics and the second poromerics is inorganic microporous material, including is micropore alumino-silicate, mesoporous silica, micro-
Hole borophosphate, aluminium phosphate molecular sieve and micropore ceramics.
3. the impurity minimizing technology of Sulfonates anionic surfactant according to claim 2, which is characterized in that institute
Stating the load of the first poromerics has cobalt chloride crystal or copper sulfate crystal or nickel sulfate hexahydrate crystal.
4. the impurity minimizing technology of Sulfonates anionic surfactant according to claim 3, which is characterized in that when
After the crystallization water that first poromerics is loaded is totally consumed, processing of living again, the place that lives again are carried out to the first poromerics
Reason includes adsorbate desorption and crystallization water generation step.
5. the impurity minimizing technology of Sulfonates anionic surfactant according to claim 1, which is characterized in that institute
The aperture for stating the second poromerics is greater than 0.45 and is less than or equal to 0.50nm, to remove alkene and alkane in product；It is described
The ratio of first poromerics and the second poromerics is 1:0.8~1:2；Described two poromerics are set using hybrid mode
It sets or subsection setup.
6. the impurity minimizing technology of Sulfonates anionic surfactant according to claim 1, which is characterized in that institute
The aperture for stating the second poromerics is 0.70-0.80nm, to remove alkylbenzene and aliphatic ester in product；Described first is micro-
The ratio of Porous materials and the second poromerics is 1:0.8~1:2；Described two poromerics are arranged using hybrid mode, or point
Section setting.
7. the impurity removal means of Sulfonates anionic surfactant, be arranged in process for sulfonation equipment discharging pipeline and at
Between product cylinder characterized by comprising
Pipeline is adsorbed, is arranged in parallel by least one adsorption tube, total caliber of the absorption pipeline is going out for process for sulfonation equipment
2~3 times of expects pipe road caliber；With
Poromerics is filled in the absorption pipeline, and loading is 0.2~1 cubic metre.
8. the impurity removal means of Sulfonates anionic surfactant according to claim 7, which is characterized in that institute
Stating poromerics includes the second poromerics of the first poromerics and aperture greater than 0.45nm that aperture is 0.40-0.45nm；
First poromerics and the second poromerics are inorganic microporous material, including micropore alumino-silicate, mesoporous silica,
Micropore borophosphate, aluminium phosphate molecular sieve and micropore ceramics；The first poromerics load has cobalt chloride crystal or copper sulphate
Crystal or nickel sulfate hexahydrate crystal.
9. the impurity removal means of Sulfonates anionic surfactant according to claim 8, which is characterized in that institute
The ratio for stating the first poromerics and second poromerics is 1:0.8~1:2；First poromerics and the first micropore
Material is filled using hybrid mode or subsection filling.
10. the impurity removal means of Sulfonates anionic surfactant according to claim 9, which is characterized in that
The aperture of second poromerics is greater than 0.45 and to be less than or equal to 0.50nm；Or the aperture of second poromerics is
0.70-0.80nm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810324774.8A CN110368715B (en) | 2018-04-12 | 2018-04-12 | Method and device for removing impurities from sulfonate anionic surfactant |
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| CN201810324774.8A CN110368715B (en) | 2018-04-12 | 2018-04-12 | Method and device for removing impurities from sulfonate anionic surfactant |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5319117A (en) * | 1989-10-28 | 1994-06-07 | Henkel Kommanditgesellschaftr Auf Aktien | Process for the sulfonation of unsaturated fatty acid glycerol esters |
| US20020197198A1 (en) * | 2001-05-04 | 2002-12-26 | Jacobson Stephen Ernest | Sulfur trioxide delivery system |
| CN102190605A (en) * | 2010-03-03 | 2011-09-21 | 北京中石大节能科技发展有限责任公司 | Petroleum sulfonate anionic surfactant and preparation method thereof |
-
2018
- 2018-04-12 CN CN201810324774.8A patent/CN110368715B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5319117A (en) * | 1989-10-28 | 1994-06-07 | Henkel Kommanditgesellschaftr Auf Aktien | Process for the sulfonation of unsaturated fatty acid glycerol esters |
| US20020197198A1 (en) * | 2001-05-04 | 2002-12-26 | Jacobson Stephen Ernest | Sulfur trioxide delivery system |
| CN102190605A (en) * | 2010-03-03 | 2011-09-21 | 北京中石大节能科技发展有限责任公司 | Petroleum sulfonate anionic surfactant and preparation method thereof |
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