CN104725541A - Preparation method of ion exchange resin for removing thermostable salt in alcohol amine solution - Google Patents
Preparation method of ion exchange resin for removing thermostable salt in alcohol amine solution Download PDFInfo
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Abstract
The invention provides a preparation method of ion exchange resin for removing thermostable salt in an alcohol amine solution. The preparation method comprises the steps that styrene, divinyl benzene, deionized water, a disperse system and an auxiliary agent are added to a polymerization kettle, and react at certain polymerization temperature; the time and speed are controlled; fine particle polystyrene white balls (particle size of 0.1-0.3mm) are obtained, cleaned, dried, and then subjected to chloromethylation; chloromethylation polystyrene resin is obtained and reacts with trimethylamine; and qualified fine particle resin is obtained. The ion exchange resin prepared by the method is small in particle size and high in specific surface area; the strong base exchange capacity is 2.9-4.7meq/g (dry agent); the efficiency of removing thermostable salt in the alcohol amine solution is improved significantly; and the elution and regeneration of the resin are easy to conduct.
Description
Technical field
The present invention relates to a kind of method of producing ion exchange resin, particularly a kind of particle thinner, the preparation method of what specific surface area was larger the remove ion exchange resin of the steady salt of heat in alkanolamine solution.
Background technology
Anionite-exchange resin can be divided into strongly basic anion exchange resin and weak base anion-exchange resin according to the character of cation exchange groups.Anionite-exchange resin intensity is high, superior performance, of many uses, can be used for the fields such as bio-chemistry separation, sewage disposal, phase-transfer catalysis reagent.
At Sweet natural gas and oil refining industry, alkanolamine solution is commonly used to remove the hydrogen sulfide in air-flow and carbonic acid gas, domestic natural gas, refinery generally adopt alkanolamine solution to carry out purifying treatment, recycle in process at alkanolamine solution and create ionic amine salt, this type of salt is in use undecomposable, be present in system, this kind of salt is called the steady salt of heat.The continuous rising of the steady salt concn of heat in alkanolamine solution, in succession occur energy consumption, amine loss increasing, the useful load of amine liquid reduces, and sweetening effectiveness is poor, and amine liquid foams, and equipment corrosion aggravates, and has influence on quality product, regeneration effect etc.
At present, domestic refinery is by regular replenishment fresh amine liquid or displacement amine liquid, but cost is larger.The employing ion exchange technique steady salt of heat removed in system is the effective ways of head it off.
US Patent No. 5788864 discloses a kind of method that ion exchange technique removes the steady salt of heat, utilize ion exchange resin commutativity to ion in the solution of different concns, constraint amine is transformed into free amine, reach the object that the steady salt of heat in amine liquid is removed, regeneration need be repeated to resin with sodium hydroxide solution, and alkali lye remaining in resin is rinsed, create waste liquid.Need reclaim amine liquid in resin bed with de-mineralized water, water-band enters system.
Chinese patent CN1861762A discloses the technology of the steady salt of a kind of ion exchange technique desuperheating, after amine liquid fluid containing the steady salt of heat flows through anion exchange resin bed, remove the steady salt of heat, adopt mode that is artificial or that automatically control to regenerate resin again, selected anionite-exchange resin is polystyrene strongly basic anion exchange resin.
Chinese patent CN2699985Y discloses a kind of gas sweetening unit amine liquid for desulphurization purification reactivating device.This device is provided with adsorption tanks, in-built weak base resin.Adsorption tanks can be composed in series by one or more.Weak base resin does not need regeneration, adopts in-line purification to bring back to life, and removes the steady salt of heat in amine liquid.
Above patented technology all uses conventional ion exchange resin, and resin particle is comparatively large, and the equipment loading resin is large, thus makes unit volume exchange capacity of resin limited, and in resin regeneration cleaning process, supplies consumption amount is large, causes wasting phenomenon.
Summary of the invention
The object of the invention is to solve existing conventional ion exchange resin, resin particle is larger, the equipment loading resin is large, thus make unit volume exchange capacity of resin limited, and in resin regeneration cleaning process, supplies consumption amount is large, causes the defect of wasting phenomenon and provides a kind of particle thinner, the preparation method of what specific surface area was larger the remove ion exchange resin of the steady salt of heat in alkanolamine solution.
To achieve these goals, the present invention is by the following technical solutions:
Remove a preparation method for the steady salt spent ion exchange resin of heat in alkanolamine solution, described preparation method comprises the following steps:
A) polyreaction: add sodium-chlor, dispersion agent, deionized water in polymeric kettle, then adds the mixing solutions of vinylbenzene and Vinylstyrene, stirs, heating is started when oil phase is dispersed into small droplets, be incubated 8h after temperature 55-75 DEG C, then continue to be warming up to 80-100 DEG C, be again incubated 12h; After question response terminates, be cooled to room temperature, filter, and wash, vacuum-drying, obtain polystyrene Archon;
B) chloromethylation: polystyrene Archon step a) obtained adds reactor, add the chloromethyl ether of polystyrene Archon 3 times of quality, then methylal is added, swelling 2-5h at 20-30 DEG C, divides and adds zinc chloride 3 times, add rear stirring 1-3h, be warming up to 35-40 DEG C, reaction 12-16h, after draining mother liquor, washing is dry, obtains chloromethylated polystyrene resin;
C) add trimethylamine solution, temperature of reaction 80-100 DEG C, reaction times 10-18h in the chloromethylated polystyrene resin obtained in step b), cooling, it is dry to take out drip washing, obtains removing the steady salt spent ion exchange resin of heat in alkanolamine solution.
As preferably, in step a), the add-on of vinylbenzene and Vinylstyrene calculates with required degree of crosslinking, and cross-linking amount is 4-10%.
As preferably, add sodium-chlor in step a), 1-3%, 0.5-2%, 15-20% that dispersion agent, deionized water are respectively vinylbenzene and Vinylstyrene total mass.
As preferably, in step a), stirring velocity is 200-500r/min.
As preferably, dispersion agent is the one in polyoxyethylene glycol, polyethylene wax, polypropylene, oxidized polyethlene wax.
As preferably, the interval that in step b), zinc chloride adds is 0.5h.
As preferably, in step b), the add-on of methylal is the 3-5% of the quality of polystyrene Archon.
As preferably, the massfraction of the trimethylamine solution added in step c) is 30%, add-on be the 2-4 of resin quality doubly.
Ion exchange resin prepared by the inventive method has following beneficial effect:
1) ion-exchange resin particles is thinner, and specific surface area is larger, and in unit volume, the highly basic exchange capacity of resin is larger, and unit volume is higher to the steady salt removal efficiency of heat in alkanolamine solution, and in equal treatment capacity situation, the volume of device resin is less, more convenient;
2) resin intermediate ion exchanges is reversible reaction fast, and fine-grained resin wash-out and regeneration are easy to carry out.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.
Method in following embodiment, if no special instructions, is the ordinary method of this area.
Embodiment 1
Remove a preparation method for the steady salt spent ion exchange resin of heat in alkanolamine solution, described preparation method comprises the following steps:
A) polyreaction
5% sodium-chlor, 2% polyoxyethylene glycol, deionized water is added in polymeric kettle, the mixing solutions of vinylbenzene and Vinylstyrene is added in polymeric kettle, degree of crosslinking is 8%, slowly start to stir, stirring velocity 200r/min, and observe, when fuel tank is dispersed into small droplets, start just to be heated to 55 ° of C and be incubated 8h, then continue to be warming up to 80 ° of C, be again incubated 12h.After polyreaction terminates, be cooled to room temperature, filter, use methyl alcohol, ethanol, deionized water wash successively, vacuum-drying, obtain polystyrene Archon; Wherein, add sodium-chlor, dispersion agent, deionized water be respectively 1%, 0.5%, 15% of vinylbenzene and Vinylstyrene total mass;
B) chloromethylation
Polystyrene Archon step a) obtained adds in reactor, add the chloromethyl ether of 3 times of polystyrene Archon quality, add 3% methylal of the quality of polystyrene Archon, swelling 2h under 20 ° of C, divides and adds zinc chloride 3 times, every minor tick 0.5h, add rear stirring 1h, be warming up to 35 ° of C, reaction 12h, after draining mother liquor resin carry out washing, dry; Obtain chloromethylated polystyrene resin.
C) functionalization
Chloromethylated polystyrene resin step c) obtained adds in reactor, add 30% trimethylamine solution of 4 times of chloromethylated polystyrene resin qualities, maintaining temperature of reaction is 80 ° of C, after reaction 10h, cooling, take out resin drip washing, drying, namely obtain removing the steady salt spent ion exchange resin of heat in alkanolamine solution, production code member DHSS-1.
Embodiment 2
Remove a preparation method for the steady salt spent ion exchange resin of heat in alkanolamine solution, described preparation method comprises the following steps:
A) polyreaction
5% sodium-chlor, 2% polyoxyethylene glycol, deionized water is added in polymeric kettle, the mixing solutions of vinylbenzene and Vinylstyrene is added in polymeric kettle, degree of crosslinking is 4%, slowly start to stir, stirring velocity 300r/min, and observe, when fuel tank is dispersed into small droplets, start just to be heated to 60 ° of C and be incubated 8h, then continue to be warming up to 90 ° of C, be again incubated 12h.After polyreaction terminates, be cooled to room temperature, filter, use methyl alcohol, ethanol, deionized water wash successively, vacuum-drying, obtain polystyrene Archon; Wherein, add sodium-chlor, dispersion agent, deionized water be respectively 2%, 1%, 18% of vinylbenzene and Vinylstyrene total mass;
B) chloromethylation
Polystyrene Archon step a) obtained adds in reactor, add the chloromethyl ether of 3 times of polystyrene Archon quality, add 4% methylal of the quality of polystyrene Archon, swelling 2.5h under 25 ° of C, divides and adds zinc chloride 3 times, every minor tick 0.5h, add rear stirring 1.5h, be warming up to 38 ° of C, reaction 14h, after draining mother liquor resin carry out washing, dry; Obtain chloromethylated polystyrene resin.
C) functionalization
Chloromethylated polystyrene resin step c) obtained adds in reactor, add 30% trimethylamine solution of 4 times of chloromethylated polystyrene resin qualities, maintaining temperature of reaction is 90 ° of C, after reaction 16h, cooling, take out resin drip washing, drying, namely obtain removing the steady salt spent ion exchange resin of heat in alkanolamine solution, production code member DHSS-2.
Embodiment 3
Remove a preparation method for the steady salt spent ion exchange resin of heat in alkanolamine solution, described preparation method comprises the following steps:
A) polyreaction
5% sodium-chlor, 2% polyoxyethylene glycol, deionized water is added in polymeric kettle, the mixing solutions of vinylbenzene and Vinylstyrene is added in polymeric kettle, degree of crosslinking is 8%, slowly start to stir, stirring velocity 400r/min, and observe, when fuel tank is dispersed into small droplets, start just to be heated to 75 ° of C and be incubated 8h, then continue to be warming up to 100 ° of C, be again incubated 12h.After polyreaction terminates, be cooled to room temperature, filter, use methyl alcohol, ethanol, deionized water wash successively, vacuum-drying, obtain polystyrene Archon; Wherein, add sodium-chlor, dispersion agent, deionized water be respectively 3%, 2%, 20% of vinylbenzene and Vinylstyrene total mass;
B) chloromethylation
Polystyrene Archon step a) obtained adds in reactor, add the chloromethyl ether of 3 times of polystyrene Archon quality, add 5% methylal of the quality of polystyrene Archon, swelling 5h under 30 ° of C, divides and adds zinc chloride 3 times, every minor tick 0.5h, add rear stirring 3h, be warming up to 40 ° of C, reaction 16h, after draining mother liquor resin carry out washing, dry; Obtain chloromethylated polystyrene resin.
C) functionalization
Chloromethylated polystyrene resin step c) obtained adds in reactor, add 30% trimethylamine solution of 4 times of chloromethylated polystyrene resin qualities, maintaining temperature of reaction is 100 ° of C, after reaction 18h, cooling, take out resin drip washing, drying, namely obtain removing the steady salt spent ion exchange resin of heat in alkanolamine solution, production code member DHSS-3.
Embodiment 4
Be polymerized stirring velocity in step a) and select 500r/min, the other the same as in Example 1.Gained removes the steady salt spent ion exchange resin of heat in alkanolamine solution, production code member DHSS-4.
Embodiment 5
In step a), the degree of crosslinking of vinylbenzene and Vinylstyrene is 4%, the other the same as in Example 1.Gained removes the steady salt spent ion exchange resin of heat in alkanolamine solution, production code member DHSS-5.
Embodiment 6
In step a), the degree of crosslinking of vinylbenzene and Vinylstyrene is 6%, the other the same as in Example 1.Gained removes the steady salt spent ion exchange resin of heat in alkanolamine solution, production code member DHSS-6.
Embodiment 7
In step a), the degree of crosslinking of vinylbenzene and Vinylstyrene is 10%, the other the same as in Example 1.Gained removes the steady salt spent ion exchange resin of heat in alkanolamine solution, production code member DHSS-7.
Embodiment 8
In step c), 30% trimethylamine solution is 2 times of chloromethylated polystyrene resin.The other the same as in Example 1.Gained removes the steady salt spent ion exchange resin of heat in alkanolamine solution, production code member DHSS-8.
Embodiment 9
In step c), 30% trimethylamine solution is 3 times of chloromethylated polystyrene resin.The other the same as in Example 1.Gained removes the steady salt spent ion exchange resin of heat in alkanolamine solution, production code member DHSS-9.
Embodiment 10 removes the steady salt capacity experimental of heat in alkanolamine solution:
In the glass ion-exchange column of diameter 50mm, long 400mm, lower end jam-pack glass cotton pad, the ion exchange resin that middle filling 300mm is high, then the amine liquid containing the steady salt of heat is added in separating funnel, open the rotory piston of ion exchange column lower end, cross post with the flow velocity of 5ml/min, after sample all flows through post, sampling analysis heat stable salts content, calculates decreasing ratio, the results are shown in Table 1:
Under the same processing condition of table 1., different resins is to heat steady salt decreasing ratio Performance comparision.
Be 5.40% containing the steady salts contg of heat in amine liquid when not crossing post
| Resin is numbered | The steady salts contg of heat in amine liquid after purification | Decreasing ratio |
| DHSS-1 | 1.60% | 70.4% |
| DHSS-2 | 1.35% | 75.0% |
| DHSS-3 | 1.10% | 79.6% |
| DHSS-4 | 0.85% | 84.3% |
| DHSS-5 | 1.05% | 80.6% |
| DHSS-6 | 1.25% | 76.9% |
| DHSS-7 | 1.80% | 66.7% |
| DHSS-8 | 1.82% | 66.3% |
| DHSS-9 | 1.95% | 63.9% |
| 201 | 2.80% | 48.1% |
| 301 | 3.40% | 37.0% |
From table 1, conventional ion exchange resin (201,301) resin particle particle size range is 0.4-1.2mm, product of the present invention removes the steady salt spent ion exchange resin grain diameter of heat in alkanolamine solution and is only 0.1-0.3mm, unit volume exchange capacity is larger, higher to the steady salt removal efficiency of heat in alkanolamine solution, resin elution and regeneration are easier to carry out, and can widely use aborning.
Claims (9)
1. remove a preparation method for the steady salt spent ion exchange resin of heat in alkanolamine solution, it is characterized in that, described preparation method comprises the following steps:
A) polyreaction: add sodium-chlor, dispersion agent, deionized water in polymeric kettle, then adds the mixing solutions of vinylbenzene and Vinylstyrene, stirs, heating is started when oil phase is dispersed into small droplets, be incubated 8h after temperature 55-75 DEG C, then continue to be warming up to 80-100 DEG C, be again incubated 12h; After question response terminates, be cooled to room temperature, filter, and wash, vacuum-drying, obtain polystyrene Archon;
B) chloromethylation: polystyrene Archon step a) obtained adds reactor, add the chloromethyl ether of polystyrene Archon 3 times of quality, then methylal is added, swelling 2-5h at 20-30 DEG C, divides and adds zinc chloride 3 times, add rear stirring 1-3h, be warming up to 35-40 DEG C, reaction 12-16h, after draining mother liquor, washing is dry, obtains chloromethylated polystyrene resin;
C) add trimethylamine solution, temperature of reaction 80-100 DEG C, reaction times 10-18h in the chloromethylated polystyrene resin obtained in step b), cooling, it is dry to take out drip washing, obtains removing the steady salt spent ion exchange resin of heat in alkanolamine solution.
2. a kind of preparation method removing the steady salt spent ion exchange resin of heat in alkanolamine solution according to claim 1, it is characterized in that, in step a), the add-on of vinylbenzene and Vinylstyrene calculates with required degree of crosslinking, and cross-linking amount is 4-10%.
3. a kind of preparation method removing the steady salt spent ion exchange resin of heat in alkanolamine solution according to claim 1, it is characterized in that, in step a), add sodium-chlor, 1-3%, 0.5-2%, 15-25% that dispersion agent, deionized water are respectively vinylbenzene and Vinylstyrene total mass.
4. a kind of preparation method removing the steady salt spent ion exchange resin of heat in alkanolamine solution according to claim 1 or 2 or 3, it is characterized in that, in step a), stirring velocity is 200-500r/min.
5. a kind of preparation method removing the steady salt spent ion exchange resin of heat in alkanolamine solution according to claim 1 or 2 or 3, it is characterized in that, dispersion agent is the one in polyoxyethylene glycol, polyethylene wax, polypropylene, oxidized polyethlene wax.
6. a kind of preparation method removing the steady salt spent ion exchange resin of heat in alkanolamine solution according to claim 1, it is characterized in that, the interval that in step b), zinc chloride adds is 0.5h.
7. a kind of preparation method removing the steady salt spent ion exchange resin of heat in alkanolamine solution according to claim 1 or 6, it is characterized in that, in step b), the add-on of methylal is the 3-5% of the quality of polystyrene Archon.
8. a kind of preparation method removing the steady salt spent ion exchange resin of heat in alkanolamine solution according to claim 1, it is characterized in that, the massfraction of the trimethylamine solution added in step c) is 30%, and add-on is 2-4 times of resin quality.
9. a kind of preparation method removing the steady salt spent ion exchange resin of heat in alkanolamine solution according to claim 1, it is characterized in that, the diameter of polystyrene Archon is 0.1-0.3mm.
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| CN106267888A (en) * | 2015-08-10 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of method removing the steady salt of heat in removal of mercaptans amine aqueous solution |
| CN107216415A (en) * | 2017-06-14 | 2017-09-29 | 中国石油化工股份有限公司 | A kind of preparation method for adsorbing the resin of anion in the steady salt of heat in amine liquid |
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| CN106267888A (en) * | 2015-08-10 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of method removing the steady salt of heat in removal of mercaptans amine aqueous solution |
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| CN107758717A (en) * | 2017-09-08 | 2018-03-06 | 中国神华能源股份有限公司 | A kind of method for liquor alumini chloridi deliming |
| CN107758717B (en) * | 2017-09-08 | 2020-03-13 | 中国神华能源股份有限公司 | Method for removing calcium from aluminum chloride solution |
| CN114522742A (en) * | 2022-02-17 | 2022-05-24 | 北京世博恒业科技有限公司 | Preparation process of desulfurization amine liquid purification resin |
| CN116832785A (en) * | 2023-05-24 | 2023-10-03 | 安庆市长三角未来产业研究院 | Graphene aerogel-ammonia modified ultrahigh crosslinked adsorption resin composite adsorption material, and preparation and application thereof |
| CN116832785B (en) * | 2023-05-24 | 2024-05-17 | 安庆市长三角未来产业研究院 | Graphene aerogel-ammonia modified ultra-high cross-linked adsorption resin composite adsorption material and its preparation and application |
| CN116808068A (en) * | 2023-06-30 | 2023-09-29 | 漆树学 | Effective substance for treating inflammatory bowel disease and preparation method thereof |
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Denomination of invention: Preparation method of ion exchange resin for removing thermally stable salts from alcohol amine solution Granted publication date: 20180309 Pledgee: Hangzhou High-tech Financing Guarantee Co.,Ltd. Pledgor: HANGZHOU DUONENG ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. Registration number: Y2024330000931 |