CN101648898B - Membrane concentration process of dimehypo mother liquor - Google Patents
Membrane concentration process of dimehypo mother liquor Download PDFInfo
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- CN101648898B CN101648898B CN2009101835801A CN200910183580A CN101648898B CN 101648898 B CN101648898 B CN 101648898B CN 2009101835801 A CN2009101835801 A CN 2009101835801A CN 200910183580 A CN200910183580 A CN 200910183580A CN 101648898 B CN101648898 B CN 101648898B
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Abstract
The invention discloses a membrane concentration process of dimehypo mother liquor. The process comprises the following steps: carrying out primary hyperfiltration and secondary nanofiltration of dimehypo mother liquor separated in a production process of monosultap to obtain concentrated liquor with the dimehypo content of 29-50 percent by weight; crystallizing the concentrated liquor and carrying out solid-liquid separation to obtain monosultap solid and high-content dimehypo liquid. The powder rate of secondary monosultap obtained by the process is 5-30 percent, and the total powder rate can reach about 78 percent. The weight content of the dimehypo in the obtained dimehypo mother liquor is 29-50 percent, and the content of sodium chloride is 2-10 percent.
Description
Technical field
The present invention relates to a kind of concentration technology of Chemicals, be specifically related to a kind of embrane method concentration technology of disosultap mother liquor.
Background technology
Disosultap and desinsection list are a kind of organic nereistoxin line sterilants, have the characteristics of efficient, low toxicity, wide spectrum.Obtain desinsection list finished product and disosultap mother liquor by raw materials such as propenyl chloride, n n dimetylaniline through operation such as amination, acidifying, dehydration, chlorination, sulfonation, crystallization, separation; Flour extraction rate of desinsection list synthesis technique is about 58% at present; All the other are centrifuge mother liquor; Disosultap weight content in the centrifuge mother liquor is 15～25%, sodium chloride content is 5～20%; Conventional treatment method is mother liquor pH to be transferred to be made into 18% dimehypo water solution after 6.5～7.5 and sell; Domestic YO reaches 100,000 tons, exist at present cause because of the aqua effective content is low packing cost high big with transportation cost, because of seasonality use cause storage pressure big, because of the aqua effective content low with contain that salinity is high possibly to cause environmental pollution such as soil salinization, the ordinary production that has restricted disosultap and desinsection list develops.
Summary of the invention
Technical problem to be solved by this invention provides a kind of embrane method concentration technology of disosultap mother liquor, and this method can produce the high-load desinsection biliquid of low salt.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following:
A kind of embrane method concentration technology of disosultap mother liquor, this method may further comprise the steps:
(1) the disosultap mother liquor with spinning gained in the desinsection list production process is collected into the mother liquor case, reaches the water inlet requirement of ultra-filtration membrane device through pre-treatment;
(2) the disosultap mother liquor that meets into water requirement is through the ultra-filtration membrane apparatus processes, and ultrafiltration and concentration liquid returns the mother liquor case, and ultrafiltration sees through liquid and gets into one-level nf membrane device;
(3) ultrafiltration sees through liquid through one-level nf membrane apparatus processes, when the mass percent concentration of disosultap in the one-level nanofiltration liquid concentrator reaches 29～50%, is collected into the liquid concentrator case, and the one-level nanofiltration sees through liquid and gets into secondary nf membrane device;
(4) the one-level nanofiltration sees through liquid through secondary nf membrane apparatus processes, and secondary nanofiltration liquid concentrator returns the import of one-level nf membrane device, and the secondary nanofiltration sees through liquid qualified discharge or as process water after biochemical treatment;
(5) with the liquid concentrator of collecting in the liquid concentrator case through crystallization and solid-liquid separation, desinsection list solid and desinsection biliquid.
In the step (1), described pre-treatment is filtered for adopting filter element filtering or filter bag, and its filtering accuracy is 0.5～100 μ m.
In the step (1), the water inlet of ultra-filtration membrane device require be: limpid, do not have mechanical impurity, no solid particulate, a concentration homogeneous.
In the step (2), described ultra-filtration membrane device is tubular fibre formula, tubular type, rolling or board-like ultra-filtration membrane device, and the ultra-filtration membrane molecular weight cut-off is 10,000～500,000 dalton.Be preferably tubular fibre formula ultra-filtration membrane device, the ultra-filtration membrane molecular weight cut-off is 100,000 dalton.
In the step (3), described one-level nf membrane device is rolling, tubular type or board-like nf membrane device, and the nf membrane molecular weight cut-off is 200～800 dalton.Be preferably rolling nf membrane device, the molecular weight cut-off of nf membrane is 300 dalton.
In the step (4), described secondary nf membrane device is rolling, tubular type or board-like nf membrane device, and the nf membrane molecular weight cut-off is 100～300 dalton.Be preferably rolling nf membrane device, the molecular weight cut-off of nf membrane is 200 dalton.
The disosultap content that sees through liquid when the secondary nanofiltration is when 3% (w/w) is above, and whole process system can connect three grades of nanofiltration device again.Being about to step (4) replaces with: the one-level nanofiltration sees through liquid through secondary nf membrane apparatus processes; Secondary nanofiltration liquid concentrator returns the import of one-level nf membrane device; The secondary nanofiltration sees through liquid through three grades of nf membrane apparatus processes; Three grades of nanofiltration liquid concentrators return the import of secondary nf membrane device, and three grades of nanofiltrations see through liquid qualified discharge or as process water after biochemical treatment.
In the step (4), described three grades of nf membrane devices are rolling, tubular type or board-like nf membrane device, and the nf membrane molecular weight cut-off is 100～200 dalton.Be preferably rolling nf membrane device, the molecular weight cut-off of nf membrane is 100 dalton.
Above-mentioned technology can adopt PLC to control automatically.
Above-mentioned ultrafiltration or nanofiltration treatment process carry out under 0～45 ℃, and gained secondary desinsection list flour extraction rate is at 5～30% (w/w) after above-mentioned process method is handled, and total flour extraction rate can reach about 78% (w/w); Gained secondary disosultap mother liquor weight content is at 29～50% (w/w), and sodium chloride content is at 2～10% (w/w).
Beneficial effect: remarkable advantage of the present invention is:
1, the inventive method energy consumption is little, adopts the embrane method concentrating unit, only needs to use electric energy.
2, the inventive method working temperature is low, only needs under 0～45 ℃ of condition, to have avoided the decomposition of active substance under the high temperature.
3, the inventive method is environmental protection, can realize cleaner production.
4, the inventive method is brought up to desinsection list flour extraction rate about 78% from original about 58%, and successfully produces the desinsection biliquid of high density, greatly facilitates production, packing, storage, transportation and the use of disosultap, has practiced thrift cost, has protected environment.
Description of drawings
Fig. 1 is the schematic flow sheet of secondary nanofiltration system of the present invention.
Fig. 2 is the schematic flow sheet of three grades of nanofiltration system of the present invention.
Embodiment:
According to following embodiment, can understand the present invention better.Yet, those skilled in the art will readily understand that the described concrete material proportion of embodiment, processing condition and result thereof only are used to explain the present invention, and the present invention that should also can not limit in claims to be described in detail.
Embodiment 1: the leading indicator of treating spissated disosultap mother liquor.
The leading indicator of treating spissated disosultap mother liquor is following:
1, disosultap: 15～25% (w/w),
2, sodium-chlor: 9% (w/w),
3, Sulfothiorine: 1.2% (w/w),
4, pH value: 5～6.
Embodiment 2: the ultra filtering clarifying system.
The disosultap mother liquor is handled through pre-filtering; Make feed liquid reach the requirement that gets into the ultra-filtration membrane device; Again through the ultra filtering clarifying art breading; Mechanical impurity wherein, suspended substance, pigment impurity etc. get fully and remove, and make the later liquid that sees through of ultra filtering clarifying not have the naked eyes visible, can guarantee the security implementation of follow-up concentration technology.
What adopt in the present embodiment is that molecular weight cut-off is the polypropylene hollow fiber microfiltration membrane of 100000Dalton; System comprises equipment such as transferpump, ultra-filtration equipment, cleaning system; Have floor space little, characteristics such as complete convenience, feed liquid good purification, level of automation height are installed.That this ultra-filtration membrane has is withstand voltage, anti-pollution, be prone to characteristics such as cleaning, long service life, and can guarantee the clarity of clear liquid for a long time, and suspended particle, colloid, organic macromolecule, bacterium, mikrobe etc. are had good separating power.Also can select the hollow-fibre membrane or the tubular membrane of other materials (like polysulfones, polyethersulfone, SE, pvdf etc.) for use.
Ultra-filtration equipment adopts the automatic operation scheme of cross flow filter, can adopt the external-compression type operation scheme.Clean the mode that adopts regular matting, recover membrane flux to greatest extent.
The ultrafiltration and concentration liquid that after ultra-filtration equipment is handled, obtains returns the mother liquor case, and ultrafiltration sees through liquid and gets into one-level nf membrane device.
Embodiment 3: one-level nanofiltration concentration systems.
One-level nanofiltration concentration systems main task is disosultap mother liquor clear liquor (being the liquid that sees through that obtains after the ultrafiltration) to be concentrated into effective constituent concentration (referring to disosultap) reach more than 29%; Through crystallization and solid-liquid separation; Wherein solid is the desinsection list, and liquid is high-load desinsection biliquid.Nanofiltration sees through liquid and then goes the secondary concentration systems to reclaim disosultap wherein.
The nf membrane that present embodiment adopts is that molecular weight cut-off is the concentrated special-purpose rolling nf membrane of 300Dalton, and operating pressure is 3.0-3.5MPa, and the average film flux is 5-15L/m
2.h..Also can select molecular weight cut-off for use is rolling or the tubular type nf membrane element of 200-800Dalton, and mould material can be polymeric amide, poly(urea formaldehyde) or Z 150PH etc.
Present embodiment respectively passes in and out the significant parameter of feed liquid:
1, feeding liquid:
1. disosultap concentration: about 20% (w/w),
2. pH value: 5.4,
3. electricity is led: 240000 μ s/cm.
2, liquid concentrator:
1. disosultap concentration is approximately: 29% (w/w),
2. pH value: 5.3,
3. electricity is led: 270000 μ s/cm.
3, see through liquid:
1. disosultap concentration is approximately: 15% (w/w),
2. pH value: 5.3,
3. electricity is led: 200000 μ s/cm.
Embodiment 4: secondary nanofiltration concentration systems.
Still contain 10～15% disosultap because one-level nanofiltration concentration systems sees through in the liquid,, lose huge if do not reclaim.Therefore, secondary nanofiltration concentration systems main task is that the liquid that sees through with the one-level nanofiltration concentrates, and the disosultap concentration of disosultap concentration and one-level charging is approaching in the control liquid concentrator, and secondary nanofiltration liquid concentrator is back to one-level nanofiltration device water-in.The disosultap concentration that the secondary nanofiltration sees through liquid lower (generally having only below 3% (w/w)); Can be disposed to environment treating facility handles; If need further to reclaim disosultap, only three grades of nanofiltration concentration technologies need be set again and get final product, as shown in Figure 2; Three grades of nanofiltration liquid concentrators return the import of secondary nf membrane device, and three grades of nanofiltrations see through liquid qualified discharge or as process water after biochemical treatment.
The nf membrane that present embodiment adopts is that molecular weight cut-off is the concentrated special-purpose rolling nf membrane of 200Dalton, and operating pressure is 3.0-3.5MPa, and the average film flux is 5-15L/m
2.h..Also can select molecular weight cut-off for use is rolling or the tubular type nf membrane element of 100-300Dalton, and mould material can be polymeric amide, poly(urea formaldehyde) or Z 150PH etc.
Present embodiment respectively passes in and out the significant parameter of feed liquid:
1, feeding liquid:
1. disosultap concentration: about 15% (w/w),
2. pH value: 5.3,
3. electricity is led: 200000 μ s/cm.
2, liquid concentrator:
1. disosultap concentration: about 20% (w/w),
2. pH value: 5.3,
3. electricity is led: 250000 μ s/cm.
3, see through liquid:
1. disosultap concentration is approximately: 3% (w/w),
2. pH value: 5.3,
3. electricity is led: 100000 μ s/cm.
Adopt above-mentioned process combination, the disosultap mother liquor that production plant comes out finally concentrates becomes the liquid concentrator of disosultap more than 29% (w/w), and through crystallization and solid-liquid separation, wherein solid is the desinsection list, and liquid is high-load desinsection biliquid.Nanofiltration can be lower than 3% (w/w) through disosultap in the liquid, and can reduce to as required below 1% (w/w).The recovery of desinsection list reaches more than 97% (w/w).
Concentrate because this technological process is a normal temperature, do not have phase transformation, the product degraded of therefore having avoided the evaporation concentration of heating usually to cause simultaneously for enterprise has saved steam, can be created certain economic benefits.
Embodiment 1～4, and disosultap mother liquor treatment capacity is 40m
3/ d, it is about 15 yuan that feed liquid per ton concentrates cost.
The data area of the foregoing description and each concrete selection are the preferred versions that is based upon on the abundant pilot scale basis, under the prerequisite that guarantees treatment effect, good economic benefits and environmental benefit are arranged.
Claims (4)
1. the embrane method concentration technology of a disosultap mother liquor is characterized in that this method may further comprise the steps:
(1) the disosultap mother liquor with spinning gained in the desinsection list production process is collected into the mother liquor case, reaches the water inlet requirement of ultra-filtration membrane device through pre-treatment;
(2) the disosultap mother liquor that meets into water requirement is through the ultra-filtration membrane apparatus processes, and ultrafiltration and concentration liquid returns the mother liquor case, and ultrafiltration sees through liquid and gets into one-level nf membrane device;
(3) ultrafiltration sees through liquid through one-level nf membrane apparatus processes, when the mass percent concentration of disosultap in the one-level nanofiltration liquid concentrator reaches 29～50%, is collected into the liquid concentrator case, and the one-level nanofiltration sees through liquid and gets into secondary nf membrane device;
(4) the one-level nanofiltration sees through liquid through secondary nf membrane apparatus processes, and secondary nanofiltration liquid concentrator returns the import of one-level nf membrane device, and the secondary nanofiltration sees through liquid qualified discharge or as process water after biochemical treatment;
(5) with the liquid concentrator of collecting in the liquid concentrator case through crystallization and solid-liquid separation, desinsection list solid and desinsection biliquid;
In the step (1), described pre-treatment is filtered for adopting filter element filtering or filter bag, and its filtering accuracy is 0.5～100 μ m;
In the step (2), described ultra-filtration membrane device is tubular fibre formula, tubular type, rolling or board-like ultra-filtration membrane device, and the ultra-filtration membrane molecular weight cut-off is 10,000～500,000 dalton;
In the step (3), described one-level nf membrane device is rolling, tubular type or board-like nf membrane device, and the nf membrane molecular weight cut-off is 200～800 dalton;
In the step (4), described secondary nf membrane device is rolling, tubular type or board-like nf membrane device, and the nf membrane molecular weight cut-off is 100～300 dalton.
2. the embrane method concentration technology of disosultap mother liquor according to claim 1 is characterized in that described ultra-filtration membrane device is a tubular fibre formula ultra-filtration membrane device, and the ultra-filtration membrane molecular weight cut-off is 100,000 dalton.
3. the embrane method concentration technology of disosultap mother liquor according to claim 1; It is characterized in that step (4) replaces with; The one-level nanofiltration sees through liquid through secondary nf membrane apparatus processes, and secondary nanofiltration liquid concentrator returns the import of one-level nf membrane device, and the secondary nanofiltration sees through liquid through three grades of nf membrane apparatus processes; Three grades of nanofiltration liquid concentrators return the import of secondary nf membrane device, and three grades of nanofiltrations see through liquid qualified discharge or as process water after biochemical treatment;
Three grades of nf membrane devices described in the step (4) are rolling, tubular type or board-like nf membrane device, and the nf membrane molecular weight cut-off is 100～200 dalton.
4. according to the embrane method concentration technology of any described disosultap mother liquor in the claim 1 to 3, it is characterized in that this process using PLC controls automatically.
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| CN105918280A (en) * | 2016-06-20 | 2016-09-07 | 安徽科发信息科技有限公司 | Light-induction electric-shock insect killing device |
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| CN102161547B (en) * | 2011-01-18 | 2012-08-08 | 中国中化股份有限公司 | Method for pretreating 2-dimethylamino-1,3-bis(sodium thiosulfate)propane production wastewater |
| CN103127833A (en) * | 2013-02-05 | 2013-06-05 | 山东兆光色谱分离技术有限公司 | Nanofiltration membrane system applied to fermented liquid purification |
| CN103537192A (en) * | 2013-10-25 | 2014-01-29 | 上海珺领生化科技有限公司 | Membrane integration device for purifying and concentrating Ertapenem aqueous solution |
| CN105621532B (en) * | 2014-10-29 | 2018-07-17 | 浙江海森药业股份有限公司 | A kind of method and application using Nanofiltration-membrane technique processing ulcerlmin crystalline mother solution and by-product sucrose octasulfate |
| CN106277521B (en) * | 2016-08-30 | 2019-07-02 | 杭州上拓环境科技股份有限公司 | A kind of dimehypo recycling mother solution reclaiming system and technique based on membrane technology |
| DK3351110T3 (en) * | 2017-01-22 | 2020-05-25 | Dmk Deutsches Milchkontor Gmbh | PROCEDURE FOR COMBINED RECOVERY OF SOUTH WHEEL AND Lactic Acid From Sour Whale |
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|---|---|---|---|---|
| CN1278403A (en) * | 2000-07-10 | 2001-01-03 | 溧阳市化工厂 | High-efficiency preparation of high-purity bisultap powder |
| CN1685818A (en) * | 2005-04-21 | 2005-10-26 | 段儒华 | Simplified production technology of bisultap |
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