CN106824305A - A kind of manufacture method and its equipment of powder anion exchange resin - Google Patents
A kind of manufacture method and its equipment of powder anion exchange resin Download PDFInfo
- Publication number
- CN106824305A CN106824305A CN201510858910.8A CN201510858910A CN106824305A CN 106824305 A CN106824305 A CN 106824305A CN 201510858910 A CN201510858910 A CN 201510858910A CN 106824305 A CN106824305 A CN 106824305A
- Authority
- CN
- China
- Prior art keywords
- kettle
- washing
- amination
- chloromethylation
- temperature
- 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.)
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 title claims abstract description 13
- 239000003957 anion exchange resin Substances 0.000 title claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 238000007265 chloromethylation reaction Methods 0.000 claims abstract description 24
- 238000005576 amination reaction Methods 0.000 claims abstract description 22
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims abstract description 20
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 18
- 239000000460 chlorine Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000008961 swelling Effects 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 4
- -1 intakes again Substances 0.000 claims abstract description 4
- 239000006210 lotion Substances 0.000 claims abstract description 4
- 239000012452 mother liquor Substances 0.000 claims abstract description 4
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 230000006641 stabilisation Effects 0.000 claims abstract description 4
- 238000011105 stabilization Methods 0.000 claims abstract description 4
- 238000010792 warming Methods 0.000 claims abstract description 4
- 239000011347 resin Substances 0.000 claims description 25
- 229920005989 resin Polymers 0.000 claims description 25
- 241001566735 Archon Species 0.000 claims description 9
- 238000013019 agitation Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- HRQGCQVOJVTVLU-UHFFFAOYSA-N bis(chloromethyl) ether Chemical compound ClCOCCl HRQGCQVOJVTVLU-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/08—Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/12—Macromolecular compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention a kind of manufacture method and its equipment of powder anion exchange resin, including mechanical crusher, chloromethylation kettle, chlorine ball washing kettle, aminating reaction kettle, amination washing kettle, washing filter, the 150um of mechanical crushing raw material size 30；Product puts into chloromethylation kettle, and swelling 2h, 20 25 DEG C of swelling temperature, 40 50 DEG C of reaction temperature is incubated 12h；Under expect chlorine ball washing kettle, wash agitation, temperature is less than 25 DEG C；Stirring expands 1h, 20 25 DEG C of temperature, plus trimethylamine temperature and is less than 35 DEG C to aminating reaction kettle, and time 10h, the 500kg/h of flow velocity 50 are warming up to 38 40 DEG C, are incubated 6h；Under expect amination washing kettle, press amination mother liquor 2h, water inlet stirring press dry water lotion, intakes again, and hydrochloric acid, stabilization 1h is added dropwise；To washing filter, pH is neutral for water inlet cleaning, discharging, present device simple structure, simple production process for blanking.
Description
Technical field
The present invention relates to resins synthesis technical field, more particularly to a kind of manufacture method and its equipment of powder anion exchange resin.
Background technology
Ion exchange resin is with functional group, with network structure, insoluble macromolecular compound.Its major part is used for water treatment field, for the removal of various zwitterions in water.The non-compliant gel or macropore negative resin or Archon less than 0.3mm or more than 1.2mm of particle diameter can be filtered out during it is produced, dangerous waste treatment is done, it is per ton to need to pay 4000 yuan, costly, the wasting of resources.Inferior gel or macropore negative resin or Archon resource less than 0.3mm or more than 1.2mm is produced powdex by this method using it, is economized on resources, with preferable economy, environmental and social benefits.
Powdex is the same with ordinary resin, from nuclear power station to sugar manufacturing industry, there is multiple use.It can be that individually sun or resin anion (R.A.) are used, it is also possible to matched according to certain Yin/Yang and mixed, be i.e. powder mixed-bed resin, directly used.
One most important characteristic of powder mixed-bed resin is to form floccule.When powdex granularity is less than 50um, the gravitation between negative resin and positive resin is dramatically increased.Porous floccule is suspended and formed in water, and volume is original 3-8 times.The volume of floccule is relevant with negative resin/positive resin proportioning.
The operating capacity of powdex unit mass is big, and the operating capacity of conventional particles resin, when failpoint is run to, is generally only the 20%~50% of theoretical exchange capacity;Powdex operating capacity reaches the 60%~95% of resin theory exchange capacity when failpoint is run to.
The ion-exchange speed of powdex is more than 100 times of ordinary resin, and because of its floccule characteristic, it is also possible to as electrostatic filter.
Powdex has good coating in filter element, and water can at a high speed pass through in the case where droop loss is little.
The content of the invention
The present invention is to provide a kind of reuse method of the non-compliant gel or macropore negative resin or Archon less than 0.3mm or more than 1.2mm of the particle diameter being screened in ion exchange resin production process.
The technical solution adopted for the present invention to solve the technical problems is：A kind of manufacturing equipment of powder anion exchange resin, including mechanical crusher, chloromethylation kettle, chlorine ball washing kettle, aminating reaction kettle, amination washing kettle, washing filter, the washing filter is connected with mechanical crusher, chloromethylation kettle is connected with chlorine ball washing kettle, the chlorine ball washing kettle is connected with aminating reaction kettle, the aminating reaction kettle is connected with amination washing kettle, and amination washing kettle is connected with washing filter.
Powdered ion-exchange resin production technology using the design is as follows：
S1：It is 30-150um by mechanical crusher mechanical crushing gel or macropore negative resin or Archon size；S2：When the product of step S1 is put into chloromethylation kettle, first swelling 2h, swelling temperature is 20-25 DEG C, and reaction temperature is 40-50 DEG C, is incubated 12h；S3：After step S2 is terminated through the reaction of chlorine ball, under expect chlorine ball washing kettle, repeated washing stirring, temperature control is below 25 DEG C；S4：By step S3 products pump stirring to aminating reaction kettle, 1h is expanded, the resin after expansion is added trimethylamine temperature control below 35 DEG C by temperature control at 20-25 DEG C, and the time is 10h, flow velocity 50-500kg/h, after trimethylamine is added, be warming up to 38-40 DEG C, be incubated 6h；S5：Amination washing kettle is expected under the product of step S4, amination mother liquor 2h is pressed, water inlet stirring press dry water lotion, intakes again, and hydrochloric acid, stabilization 1h is added dropwise；S6：By step S5 products blanking to washing filter, water inlet cleaning seven times, discharging neutral to pH.Preferably, the chloromethylation kettle temperature degree is 40 DEG C, and aminating reaction kettle temperature degree is 30 DEG C.
Preferably, the chloromethylation kettle temperature degree is 42 DEG C, and aminating reaction kettle temperature degree is 33 DEG C.
Preferably, the chloromethylation kettle temperature degree is 45 DEG C, and aminating reaction kettle temperature degree is 35 DEG C.
Beneficial effect：Inferior gel or macropore negative resin or Archon resource less than 0.3mm or more than 1.2mm is produced powdex by this equipment using it, is economized on resources, and with preferable economy, environmental and social benefits, this device structure is simple, and production procedure is easily controllable.
Brief description of the drawings
Fig. 1 is structural representation of the invention.
Wherein：1. the amination washing kettle of 2. mechanical crusher of washing filter, 3. chloromethylation kettle, 4. 5. aminating reaction kettle of chlorine ball washing kettle 6..
Specific embodiment
One embodiment is described below in conjunction with the accompanying drawings, and the invention will be further described.
Embodiment 1：In figure, a kind of manufacturing equipment of powder anion exchange resin, including mechanical crusher, chloromethylation kettle, chlorine ball washing kettle, aminating reaction kettle, amination washing kettle, washing filter, the washing filter is connected with mechanical crusher, chloromethylation kettle is connected with chlorine ball washing kettle, the chlorine ball washing kettle is connected with aminating reaction kettle, and the aminating reaction kettle is connected with amination washing kettle, and amination washing kettle is connected with washing filter.
Powdered ion-exchange resin production technology using the design is as follows：
S1：It is 30-150um by mechanical crusher mechanical crushing gel or macropore negative resin or Archon size；S2：When the product of step S1 is put into chloromethylation kettle, first swelling 2h, swelling temperature is 20-25 DEG C, and reaction temperature is 40-50 DEG C, is incubated 12h；S3：After step S2 is terminated through the reaction of chlorine ball, under expect chlorine ball washing kettle, repeated washing stirring, temperature control is below 25 DEG C；S4：By step S3 products pump stirring to aminating reaction kettle, 1h is expanded, the resin after expansion is added trimethylamine temperature control below 35 DEG C by temperature control at 20-25 DEG C, and the time is 10h, flow velocity 50-500kg/h, after trimethylamine is added, be warming up to 38-40 DEG C, be incubated 6h；S5：Amination washing kettle is expected under the product of step S4, amination mother liquor 2h is pressed, water inlet stirring press dry water lotion, intakes again, and hydrochloric acid, stabilization 1h is added dropwise；S6：By step S5 products blanking to washing filter, water inlet cleaning seven times, discharging neutral to pH.
In chloromethylation Amination Technique flow, in 5000L chloromethylations kettle 3, powdex reacts under catalyst action with chloromethyl ether, reaction temperature is 40 DEG C, in 5000L aminating reactions kettle 4, the resin after expansion reacts with trimethylamine, and reaction temperature is 30 DEG C.
Embodiment 2：In chloromethylation Amination Technique flow, in 5000L chloromethylations kettle 3, Archon reacts under catalyst action with chloromethyl ether, and reaction temperature is 42 DEG C, and in 5000L aminating reactions kettle 4, the resin after expansion reacts with trimethylamine, and reaction temperature is 33 DEG C.
Embodiment 3：In chloromethylation Amination Technique flow, in 5000L chloromethylations kettle 3, Archon reacts under catalyst action with chloromethyl ether, and reaction temperature is 45 DEG C, and in 5000L aminating reactions kettle 4, the resin after expansion reacts with trimethylamine, and reaction temperature is 35 DEG C.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the invention is limited; equivalent structure or equivalent flow conversion that all utilization description of the invention and accompanying drawing content are made; or other related technical fields are directly or indirectly used in, it is included within the scope of the present invention.
Claims (5)
1. a kind of manufacturing equipment of powder anion exchange resin, it is characterised in that：Including mechanical crusher, chloromethylation kettle, chlorine ball washing kettle, aminating reaction kettle, amination washing kettle, washing filter, the washing filter is connected with mechanical crusher, chloromethylation kettle is connected with chlorine ball washing kettle, the chlorine ball washing kettle is connected with aminating reaction kettle, the aminating reaction kettle is connected with amination washing kettle, and amination washing kettle is connected with washing filter.
2. the method that powder anion exchange resin is manufactured using device as claimed in claim 1, it is characterized in that, S1：It is 30-150um by mechanical crusher mechanical crushing gel or macropore negative resin or Archon size；S2：When the product of step S1 is put into chloromethylation kettle, first swelling 2h, swelling temperature is 20-25 DEG C, and reaction temperature is 40-50 DEG C, is incubated 12h；S3：After step S2 is terminated through the reaction of chlorine ball, under expect chlorine ball washing kettle, repeated washing stirring, temperature control is below 25 DEG C；S4：By step S3 products pump stirring to aminating reaction kettle, 1h is expanded, the resin after expansion is added trimethylamine temperature control below 35 DEG C by temperature control at 20-25 DEG C, and the time is 10h, flow velocity 50-500kg/h, after trimethylamine is added, be warming up to 38-40 DEG C, be incubated 6h；S5：Amination washing kettle is expected under the product of step S4, amination mother liquor 2h is pressed, water inlet stirring press dry water lotion, intakes again, and hydrochloric acid, stabilization 1h is added dropwise；S6：By step S5 products blanking to washing filter, water inlet cleaning seven times, discharging neutral to pH.
3. it is according to claim 2 manufacture powder anion exchange resin method, it is characterized in that:The chloromethylation kettle temperature degree is 40 DEG C, and aminating reaction kettle temperature degree is 30 DEG C.
4. it is according to claim 2 manufacture powder anion exchange resin method, it is characterized in that:The chloromethylation kettle temperature degree is 42 DEG C, and aminating reaction kettle temperature degree is 33 DEG C.
5. it is according to claim 2 manufacture powder anion exchange resin method, it is characterized in that:The chloromethylation kettle temperature degree is 45 DEG C, and aminating reaction kettle temperature degree is 35 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510858910.8A CN106824305A (en) | 2015-12-01 | 2015-12-01 | A kind of manufacture method and its equipment of powder anion exchange resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510858910.8A CN106824305A (en) | 2015-12-01 | 2015-12-01 | A kind of manufacture method and its equipment of powder anion exchange resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106824305A true CN106824305A (en) | 2017-06-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510858910.8A Pending CN106824305A (en) | 2015-12-01 | 2015-12-01 | A kind of manufacture method and its equipment of powder anion exchange resin |
Country Status (1)
| Country | Link |
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| CN (1) | CN106824305A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112090454A (en) * | 2020-09-16 | 2020-12-18 | 浙江天顺生物科技有限公司 | Macroporous weakly-alkaline styrene anion exchange resin method and equipment thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101518747A (en) * | 2008-04-16 | 2009-09-02 | 浙江争光实业股份有限公司 | Recycling system of chlorination mother solution and recycling method thereof |
| CN101781381A (en) * | 2009-12-31 | 2010-07-21 | 安徽皖东化工有限公司 | Preparation method of 201*4 strong-basicity styrene series anion exchange resin |
| CN102557191A (en) * | 2012-02-23 | 2012-07-11 | 宁波争光树脂有限公司 | Process for synthesizing powdered ion-exchange resin |
| CN205199524U (en) * | 2015-12-01 | 2016-05-04 | 江苏金凯树脂化工有限公司 | Powder anion exchange resin's manufacture equipment |
-
2015
- 2015-12-01 CN CN201510858910.8A patent/CN106824305A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101518747A (en) * | 2008-04-16 | 2009-09-02 | 浙江争光实业股份有限公司 | Recycling system of chlorination mother solution and recycling method thereof |
| CN101781381A (en) * | 2009-12-31 | 2010-07-21 | 安徽皖东化工有限公司 | Preparation method of 201*4 strong-basicity styrene series anion exchange resin |
| CN102557191A (en) * | 2012-02-23 | 2012-07-11 | 宁波争光树脂有限公司 | Process for synthesizing powdered ion-exchange resin |
| CN205199524U (en) * | 2015-12-01 | 2016-05-04 | 江苏金凯树脂化工有限公司 | Powder anion exchange resin's manufacture equipment |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112090454A (en) * | 2020-09-16 | 2020-12-18 | 浙江天顺生物科技有限公司 | Macroporous weakly-alkaline styrene anion exchange resin method and equipment thereof |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170613 |
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| WD01 | Invention patent application deemed withdrawn after publication |