CN102816341A - Synthetic method for weak-acid adsorption resin suitable for heavy oil wastewater - Google Patents
Synthetic method for weak-acid adsorption resin suitable for heavy oil wastewater Download PDFInfo
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- CN102816341A CN102816341A CN2012103158681A CN201210315868A CN102816341A CN 102816341 A CN102816341 A CN 102816341A CN 2012103158681 A CN2012103158681 A CN 2012103158681A CN 201210315868 A CN201210315868 A CN 201210315868A CN 102816341 A CN102816341 A CN 102816341A
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Abstract
The invention relates to a synthetic method for weak-acid adsorption resin suitable for heavy oil wastewater. The synthetic method includes following steps: adding initiator into an oil phase; adding the oil phase added with the initiator into a water phase under stirring to obtain a mixture, heating up to 50 DEG C to 65 DEG C and maintaining for 6-8 hours, further heating up to 85 DEG C to 90 DEG C and maintaining for 12-15 hours, then cooling to obtain poly acrylic white balls, and extracting or cleaning for drying treatment; and subjecting the poly acrylic white balls after the drying treatment to swelling with ethanol at the temperature of 50 DEG C to 60 DEG C, mixing with sulfuric acid with a concentration of 50-70wt% at the temperature of 120 DEG C-140 DEG C for hydrolysis reaction, and then sequentially diluting, transforming and water-washing to obtain the weak-acid adsorption resin suitable for the heavy oil wastewater. The weak-acid adsorption resin synthesized by the method is quite good in resistance to organic pollution, improved in working conversion capacity and ion exchange reaction rate of the resin and suitable for serving as primary softener to adsorb most calcium and magnesium ions in the heavy oil wastewater.
Description
Technical field
The present invention relates to a kind of compound method that is applicable to the weak acid polymeric adsorbent of condensed oil sewage, belong to oil production with the synthetic field of macromolecular material.
Background technology
When being applied to the weak acid polymeric adsorbent in the condensed oil sewage; Because contain the lot of background material in the condensed oil sewage, like humic acid, vegetable and animals oils and petroleum-type etc., these materials can be adsorbed on resin surface by the oil loving skeleton of resin; Form one deck water oil mixt; Slow down metals ion in the water to the speed of resin internal divergence, make it go out water concentration and can't reduce to the ppb level, cause the reuse thermal recovery boiler to cause the problem of fouling.
The compound method of a lot of weak acid resins is provided, to improve its use properties in the prior art.CN86101585A discloses a kind of synthetic technology of resins used for acrylic weak ion exchange.Problem such as be clamminess when, when operation caking on the low side with the crosslinked existing physical strength of resins used for acrylic weak ion exchange of Vinylstyrene (DVB) in order to solve, storage; The disclosed technical scheme of this patented claim adopts the mixture of Vinylstyrene and iso-cyanuric acid triallyl ester (TAIC) to make compound linking agent; During suspension polymerization; Under the situation of not isolating a polymkeric substance; Pass through crosslinking reaction mutually mutually with a certain amount of monomer; Acrylic acid synthesizing is the skeleton of weak acid ion-exchange resin, the resin that obtains therefrom have physical strength good, do not lump, be not clamminess, advantage such as the deformation rate of expansion is low, have been widely used at aspects such as water treatment, the disposal of three wastes, pharmaceutical industry, sugar industry and hydrometallurgys.
CN101948554A discloses a kind of magnetic acrylic acid series Weak-acid cation exchange microballoon resin and compound method thereof.The compound method that this patented claim provided is carried out suspension polymerization through being magnetic-particle and the oil phase uniform mixing of 0.01-10 μ m with size under certain temperature and condition, finally form the magnetic weakly acidic cationic exchanger resin through hydrolysis.This microballoon resin is to be made up of Weak-acid cation exchange microballoon resin skeleton and the magnetic-particle that is wrapped in wherein; The weight ratio of resin matrix and magnetic-particle is 1: 0.05-1; Its weak acid volume-exchange capacity is 1.0-5.0mol/L; Median size is 20-500 μ m, and its specific saturation magnetization is 5.1-33.4emu/g, and the weak acid exchange capacity is 1.0-5.0mol/L.This microballoon resin can be used in the processing of various water bodies, removes multiple metals ions such as ammonia nitrogen and calcium, magnesium, copper, nickel, cadmium.
CN1389296A discloses a kind of preparation method of weakly acidic cationic exchanger resin.This method is to be used to clean improving one's methods of weakly acidic cationic exchanger resin midbody, and resulting weak acid resin provides has the enhanced processing property in the mixed bed water treatment system.
But the disclosed technical scheme of above-mentioned patented claim all is only to improve resin property from the physicals or the chemical property of weak acid resin, does not regulate the resin synthetic parameters to different condition of water quality and improves the application performance of resin in certain water quality.
Summary of the invention
For solving the problems of the technologies described above; The object of the present invention is to provide a kind of compound method of weak acid polymeric adsorbent; Synthetic parameters through regulating resin obtains a kind of special efficacy weak acid polymeric adsorbent that is applicable to condensed oil sewage; This weak acid polymeric adsorbent has very strong antifouling property, can in the condensed oil sewage of high organic content, efficiently remove the metals ion in the water, makes it in the reuse thermal recovery boiler, not produce scale problems.
The present invention also aims to provide above-mentioned compound method synthetic weak acid polymeric adsorbent.
For achieving the above object, the invention provides a kind of compound method that is applicable to the weak acid polymeric adsorbent of condensed oil sewage, it may further comprise the steps:
In oil phase, add the initiator that accounts for oil phase quality 1-3%, stirring is fully dissolved initiator;
The oil phase that has added initiator is added to the aqueous phase that is in the stirring; Obtain mixture, stirring velocity is controlled to be 100-300rpm, after having added; Temperature is elevated to 50-65 ℃ of insulation 6-8 hour; Be warming up to 85-90 ℃ of insulation 12-15 hour again, cooling obtains the polyacrylic Archon then, carries out drying treatment after extracting or the cleaning;
With the polyacrylic Archon after the drying treatment with ethanol in 50-60 ℃ of following swelling; Be that the sulfuric acid of 50-70wt% is blended in the 120-140 ℃ of reaction that is hydrolyzed with concentration again, again through progressively diluting, make the transition, wash (thin up, repetitive scrubbing 4-5 time; Adopting volume is 3-5 times of resin volume; Concentration is NaOH solution transition of 3-5%, after washing until neutrality), obtain being applicable to the weak acid polymeric adsorbent of condensed oil sewage;
Wherein, water is the aqueous solution that contains dispersion agent and NaCl, and in the total mass of water, the concentration of dispersion agent is 1.5-3wt%, and the concentration of NaCl is 12-20wt%;
Oil phase is made up of reactant and pore-creating agent; The mass ratio of reactant and pore-creating agent is 1: 0.45-1: 0.55; Reactant comprises acrylonitrile monemer and allyl methacrylate(AMA) linking agent, and the mass ratio of acrylonitrile monemer and propyl methacrylate linking agent is 1: 0.10-1: 0.14.
Compound method provided by the present invention is from resin organic two aspects of intercepting of organic parcel absorption and the inner duct of resin to be designed the resin compound method; Monomer, the bigger pore-creating agent of linking agent and formation aperture that the option table surface tension is minimum; Improve the hydrophilic oleophobic property of resin; Improve the oil rub resistance metachromia ability of resin through the synthetic parameters that changes resin, thereby improve operating capacity and the speed of reaction of resin in condensed oil sewage.This method synthetic weak acid polymeric adsorbent is a kind of used for acrylic weak Zeo-karb, is suitable for the processing of condensed oil sewage.
In above-mentioned compound method, preferably, the dispersion agent that aqueous phase adopted is one or more in inorganics of gelatin, Z 150PH, starch, methylcellulose gum and verivate thereof and insoluble etc.
In above-mentioned compound method, preferably, the initiator that is adopted is Lucidol or Diisopropyl azodicarboxylate etc.
In above-mentioned compound method, preferably, the pore-creating agent that is adopted is an isopropylcarbinol, 200
#In gasoline and the positive structure wet goods one or more.
In above-mentioned compound method, preferably, when swelling, polypropylene-based Archon and alcoholic acid mass ratio can be 1: 1-1: 4, more preferably 1: 2-1: 3.
In above-mentioned compound method, preferably, in hydrolysis reaction, the vitriolic addition is 0.5-2 a times of acrylonitrile monemer volume.Polyacrylic Archon and sulfuric acid can import hydroxy-acid group after being hydrolyzed and reacting on the skeleton of polyacrylic Archon.
The present invention also provides a kind of weak acid polymeric adsorbent that is applicable to condensed oil sewage, and it is by above-mentioned compound method synthetic.Preferably, the particle diameter of above-mentioned weak acid polymeric adsorbent is 0.500-1.250mm.
The compound method that is applicable to the weak acid polymeric adsorbent of condensed oil sewage provided by the present invention is to condensed oil sewage background material (like humic acid, vegetable and animals oils, petroleum-type etc.) the higher characteristics of content; Adopting a certain amount of vinyl cyanide is that monomer, allyl methacrylate(AMA) are that linking agent and isopropylcarbinol synthesize polypropylene-based Archon as pore-creating agent; With itself and the sulfuric acid hydrolysis reaction that heats up; Thereby on skeleton, import hydroxy-acid group; Through progressively diluting, make the transition, washing, finally synthesize the Weak-acid cation polymeric adsorbent again.Has good anti-Organic pollutants performance through this method synthetic weak acid polymeric adsorbent; The operating capacity and the ion exchange reaction speed of resin have been improved; Be applicable in condensed oil sewage water quality and soften the most calcium ions and magnesium ions of absorption, make it be reduced to the ppb level from the ppm level as one-level.
The compound method of weak acid polymeric adsorbent provided by the invention and weak acid polymeric adsorbent have the following advantages:
1, the compound method of compound method provided by the invention and traditional weak acid resin is similar, is easy to realize scale operation;
2, compound method provided by the invention has selected for use the wetting ability isopropylcarbinol that vinyl cyanide and allyl methacrylate(AMA) and molecular weight are bigger preferably as synthetic materials, and the oil rub resistance metachromia that can significantly improve synthetic weak acid polymeric adsorbent can;
3, the compound method provided by the invention performances such as speed of reaction, operating capacity that after confirming synthetic materials, are directed against resin absorption divalent calcium mg ion change synthetic parameters, can improve the operating capacity of this weak acid polymeric adsorbent to the divalent calcium mg ion;
4, weak acid polymeric adsorbent provided by the present invention is applicable to background material (like humic acid, vegetable and animals oils, petroleum-type etc.) the higher condensed oil sewage of content, compares with traditional weak acid resin, has good oil rub resistance metachromia ability and very high operating capacity.
Embodiment
To understand in order technical characterictic of the present invention, purpose and beneficial effect being had more clearly, technical scheme of the present invention is carried out following detailed description, but but can not be interpreted as qualification at present practical range of the present invention.
Embodiment 1
Present embodiment provides a kind of weak acid polymeric adsorbent, and it prepares through following steps:
The aqueous solution (water) of sodium-chlor that 500mL is contained gelatin, the 15wt% of 2wt% joins in the 2L there-necked flask, stirs, and stirring velocity is controlled at 100-150rpm;
100g acrylonitrile monemer, 12g allyl methacrylate(AMA) and the mixing of 45g isopropylcarbinol are obtained oil phase; Add the 1.0g Lucidol to again and mix in the oil phase, join then in the there-necked flask that contains water, keep in the time of adding stirring; Accomplish after the interpolation; Be warming up to 50 ℃ and be incubated 6 hours, and then be warming up to 85 ℃ of insulations and obtain the polyacrylic Archon, discharging after 12 hours;
Dry after with ethanol the polyacrylic Archon being cleaned; Add 2 times of ethanol and make its abundant swelling to polyacrylic Archon quality; Be that the sulfuric acid of 60wt% is blended in 140 ℃ of reactions that are hydrolyzed with the concentration of 1 times of acrylonitrile monemer volume then, thereby on skeleton, import hydroxy-acid group, thin up again; Repetitive scrubbing 4-5 time; Adopting volume is the NaOH solution transition that 3-5 times of polystyrene Archon volume, concentration are 3-5wt%, after washing until neutrality, obtains the weak acid polymeric adsorbent.
This weak acid polymeric adsorbent is a kind of weakly acidic cationic exchanger resin, and its size distribution is at 0.500-1.250mm, and the operating capacity in condensed oil sewage can reach 2.70mmol/g.
Learn from else's experience overregulate, coagulant precipitation, dissolved air floatation and the cascade filtration condensed oil sewage 50L after handling, its water-quality guideline is as shown in table 1.
Table 1
| Water sample | Total hardness (mg/L) | Calcium (mg/L) | Magnesium (mg/L) | COD(mg/L) | Temperature (℃) |
| Water inlet | 78 | 28 | 5 | 410 | 53 |
Measure 50mL present embodiment synthetic weak acid resin in adsorption column, the condensed oil sewage after handling is passed through adsorption column under the flow velocity of 20BV/h, regularly determine water concentration, its effluent index is as shown in table 2.Data in the table 2 are the equilibrium adsorption concentration before reaching the resin breakthrough point, can be found out that by the data of table 2 present embodiment synthetic weak acid resin has the good adsorption ability.
Table 2
| Water sample | Total hardness (mg/L) | Calcium (mg/L) | Magnesium (mg/L) | Adsorption cycle | COD(mg/L) | Regenerative elution rate (%) |
| Water outlet | 0.550-0.800 | 0.100-0.150 | 0.080-0.100 | 1450 | 385-400 | 99.1 |
Data by table 1 and table 2 can find out that after treatment, the total hardness of condensed oil sewage is reduced to below the 1mg/L, and calcium ions and magnesium ions concentration is lower, and have long adsorption cycle.Simultaneously, present embodiment synthetic weak acid resin is less to organic absorption, adsorbs saturated back and can reach very high organic matter regeneration eluting rate through regeneration, and present embodiment synthetic weak acid resin has higher work-ing life in condensed oil sewage.
Embodiment 2
Present embodiment provides a kind of weak acid polymeric adsorbent, and it prepares through following steps:
The aqueous solution (water) of sodium-chlor that 500mL is contained gelatin, the 20wt% of 3wt% joins in the 2L there-necked flask, stirs, and stirring velocity is controlled at 150-200rpm;
100g acrylonitrile monemer, 14g allyl methacrylate(AMA) and the mixing of 50g isopropylcarbinol are obtained oil phase; Again the 1.0g Lucidol is added to and mix in the oil phase, join then in the there-necked flask that contains water, keep in the time of adding stirring; Accomplish after the interpolation; Be warming up to 60 ℃ and be incubated 6 hours, and then be warming up to 90 ℃ of insulations and obtain the polyacrylic Archon, discharging after 12 hours;
Dry after with ethanol the polyacrylic Archon being cleaned; Add 3 times of ethanol and make its abundant swelling to polyacrylic Archon quality; Be that the sulfuric acid of 60wt% is blended in 140 ℃ of reactions that are hydrolyzed with the concentration of 0.5 times of acrylonitrile monemer volume then, thereby on skeleton, import hydroxy-acid group, thin up again; Repetitive scrubbing 4-5 time; Adopting volume is the NaOH solution transition that 3-5 times of polystyrene Archon volume, concentration are 3-5wt%, after washing until neutrality, obtains the weak acid polymeric adsorbent.
This weak acid polymeric adsorbent is a kind of weakly acidic cationic exchanger resin, and its size distribution is at 0.400-1.100mm, and the operating capacity in condensed oil sewage can reach 2.61mmol/g.
Learn from else's experience overregulate, coagulant precipitation, dissolved air floatation and the cascade filtration condensed oil sewage 50L after handling, its water-quality guideline is as shown in table 3.
Table 3
| Water sample | Total hardness (mg/L) | Calcium (mg/L) | Magnesium (mg/L) | COD(mg/L | Temperature (℃) |
| Water inlet | 102 | 38 | 11 | 360 | 54 |
Measure 50mL present embodiment synthetic weak acid resin in adsorption column, the condensed oil sewage after handling is passed through adsorption column under the flow velocity of 20BV/h, regularly determine water concentration, after absorption reaches breakthrough, stop absorption, write down volume of water.Its effluent index is as shown in table 4.
Table 4
| Water sample | Total hardness (mg/L) | Calcium (mg/L) | Magnesium (mg/L) | Adsorption cycle | COD(mg/L) | Regenerative elution rate (%) |
| Water outlet | 0.500-0.850 | 0.100-0.170 | 0.070-0.110 | 1370 | 340-350 | 98.5 |
Data by table 3 and table 4 can find out that after treatment, the total hardness of condensed oil sewage is reduced to below the 1mg/L, and calcium ions and magnesium ions concentration is lower, and have long adsorption cycle.Simultaneously, present embodiment synthetic weak acid resin is less to organic absorption, adsorbs saturated back and can reach very high organic matter regeneration eluting rate through regeneration, and present embodiment synthetic weak acid resin has higher work-ing life in condensed oil sewage.
Simultaneously; Show 1-table 4 operating capacity of embodiment 1 and 2 synthetic weak acid resins be provided, cross the difference of water front and back COD; And to the eluting rate of COD of absorption; Through these numerical value all can find out embodiment 1 and 2 synthetic weak acid resins have very high operating capacity and well the oil rub resistance metachromia can, and the effluent index of the calcium ions and magnesium ions that provides from table 1-table 4 can be found out; Adopt embodiment 1 and 2 synthetic weak acid resins that the concentration of calcium ions and magnesium ions is reduced to below the 100ppb, show that it has very strong adsorptive power to calcium ions and magnesium ions.
Claims (9)
1. compound method that is applicable to the weak acid polymeric adsorbent of condensed oil sewage, it may further comprise the steps:
In oil phase, add the initiator that accounts for oil phase quality 1-3%, stirring is fully dissolved initiator;
The oil phase that has added initiator is added to the aqueous phase that is in the stirring; Obtain mixture, stirring velocity is controlled to be 100-300rpm, after having added; Temperature is elevated to 50-65 ℃ of insulation 6-8 hour; Be warming up to 85-90 ℃ of insulation 12-15 hour again, cooling obtains the polyacrylic Archon then, carries out drying treatment after extracting or the cleaning;
With the polyacrylic Archon after the drying treatment with ethanol in 50-60 ℃ of following swelling; Be that the sulfuric acid of 50-70wt% is blended in the 120-140 ℃ of reaction that is hydrolyzed with concentration again; Through progressively diluting, make the transition, washing, obtain the said weak acid polymeric adsorbent that is applicable to condensed oil sewage again;
Wherein, said water is the aqueous solution that contains dispersion agent and NaCl, and in the total mass of water, the concentration of dispersion agent is 1.5-3wt%, and the concentration of NaCl is 12-20wt%;
Said oil phase is made up of reactant and pore-creating agent; The mass ratio of said reactant and pore-creating agent is 1: 0.45-1: 0.55; Said reactant comprises acrylonitrile monemer and allyl methacrylate(AMA) linking agent, and the mass ratio of said acrylonitrile monemer and propyl methacrylate linking agent is 1: 0.10-1: 0.14.
2. compound method according to claim 1, wherein, the dispersion agent of said aqueous phase is one or more in the inorganics of gelatin, Z 150PH, starch, methylcellulose gum and verivate thereof and insoluble.
3. compound method according to claim 1, wherein, said initiator is Lucidol or Diisopropyl azodicarboxylate.
4. compound method according to claim 1, wherein, said pore-creating agent is an isopropylcarbinol, 200
#In gasoline and the positive structure oil one or more.
5. compound method according to claim 1, wherein, when swelling, said polypropylene-based Archon and said alcoholic acid mass ratio are 1: 1-1: 4.
6. compound method according to claim 5, wherein, said polypropylene-based Archon and said alcoholic acid mass ratio are 1: 2-1: 3.
7. compound method according to claim 1, wherein, in hydrolysis reaction, the 0.5-2 that said vitriolic addition is the acrylonitrile monemer volume doubly.
8. weak acid polymeric adsorbent that is applicable to condensed oil sewage, it is by each described compound method synthetic of claim 1-7.
9. the weak acid polymeric adsorbent that is applicable to condensed oil sewage according to claim 8, wherein, this is applicable to that the particle diameter of the weak acid polymeric adsorbent of condensed oil sewage is 0.500-1.250mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884967A (en) * | 2015-08-26 | 2016-08-24 | 同济大学 | Contamination-resistant large-capacity macroporous weak-acid resin synthesis method |
| CN109369852A (en) * | 2018-10-30 | 2019-02-22 | 扬州金珠树脂有限公司 | A kind of preparation method of nickel, cobalt, polluted by copper resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829609A (en) * | 2010-05-25 | 2010-09-15 | 中蓝晨光化工研究院有限公司 | Tertiary-amino-containing macroporous anion exchange resin and preparation method thereof |
| CN101948554A (en) * | 2010-10-09 | 2011-01-19 | 南京大学 | Weak acid cation exchange microballoon resin of magnetic acrylic acid series and synthesis method thereof |
| CN102234353A (en) * | 2011-04-20 | 2011-11-09 | 安徽美佳新材料股份有限公司 | Preparation method of D113 dilute acid acrylic cation-exchange resin |
-
2012
- 2012-08-30 CN CN2012103158681A patent/CN102816341A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829609A (en) * | 2010-05-25 | 2010-09-15 | 中蓝晨光化工研究院有限公司 | Tertiary-amino-containing macroporous anion exchange resin and preparation method thereof |
| CN101948554A (en) * | 2010-10-09 | 2011-01-19 | 南京大学 | Weak acid cation exchange microballoon resin of magnetic acrylic acid series and synthesis method thereof |
| CN102234353A (en) * | 2011-04-20 | 2011-11-09 | 安徽美佳新材料股份有限公司 | Preparation method of D113 dilute acid acrylic cation-exchange resin |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884967A (en) * | 2015-08-26 | 2016-08-24 | 同济大学 | Contamination-resistant large-capacity macroporous weak-acid resin synthesis method |
| CN105884967B (en) * | 2015-08-26 | 2018-08-31 | 同济大学 | A kind of synthetic method of anti-pollution type large capacity Macroporous Weakly-Acid |
| CN109369852A (en) * | 2018-10-30 | 2019-02-22 | 扬州金珠树脂有限公司 | A kind of preparation method of nickel, cobalt, polluted by copper resin |
| CN109369852B (en) * | 2018-10-30 | 2021-03-23 | 扬州金珠树脂有限公司 | Preparation method of nickel, cobalt and copper adsorption resin |
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