CN108706751A - A kind of research of non-phosphorus scale inhibitor and preparation method thereof - Google Patents
A kind of research of non-phosphorus scale inhibitor and preparation method thereof Download PDFInfo
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- CN108706751A CN108706751A CN201810790338.XA CN201810790338A CN108706751A CN 108706751 A CN108706751 A CN 108706751A CN 201810790338 A CN201810790338 A CN 201810790338A CN 108706751 A CN108706751 A CN 108706751A
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- research
- scale inhibitor
- stirring
- phosphorus scale
- cyclodextrin
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
- C02F5/12—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
- C08G65/2621—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
- C08G65/263—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups containing heterocyclic amine groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- General Chemical & Material Sciences (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention relates to a kind of research of non-phosphorus scale inhibitor and preparation method thereof, and its step are as follows：(1) cyclodextrin, the vinyl ethers with amino, water are added into stirring-type polymer reactor, opens stirring, and begin to warm up heating；(2) when the temperature in stirring-type polymer reactor rises to 105 DEG C~135 DEG C, start that the initiator solution that mass concentration is 1~7% is added dropwise, this initiator solution is formulated by the initiator and the part water, and time for adding was controlled at 3~6 hours；(3) after dripping, then epoxychloropropane is added in stirring-type polymer reactor, keeping temperature, the reaction was continued 1~3 hour, and cooling discharge is to get the research of non-phosphorus scale inhibitor.
Description
Technical field
The invention belongs to industrial water conditioning agent technical field, more particularly to a kind of research of non-phosphorus scale inhibitor and preparation method thereof.
Background technology
Antisludging agent is important one of water treatment agent, slightly solubility inorganic salts that it can be in score water inhibit or interfere with
The slightly solubility inorganic salts precipitation that metal shows again, maintains metal equipment to have good heat-transfer effect at structure function.Domestic at present
Antisludging agent has organic phosphates antisludging agent, organic phosphate antisludging agent, polycarboxylic acid dirt dispersion agent, synthetic polymer scale inhibition
Agent, RO (reverse osmosis) antisludging agent etc..Antisludging agent is used in boiler feed water and cooling water in the industrial production, can prevent from exchanging heat
Equipment scaling and corrosion improve heat conduction efficiency, reduce energy consumption and maintenance cost, extend service life of equipment.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of research of non-phosphorus scale inhibitor and preparation method thereof, should
Research of non-phosphorus scale inhibitor has good scale-inhibiting properties, and not phosphorous, directly avoids phosphorus-containing wastewater discharge that Water Eutrophication is caused to ask
Topic.
To achieve the goals above, the present invention uses following technical scheme：
A kind of research of non-phosphorus scale inhibitor, the raw material components matched by following mass fractions are made：
The cyclodextrin is that one or more of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin are mixed with arbitrary ratio
The mixture of conjunction.
The vinyl ethers with amino are 2- amino-ethyls vinyl ethers, 3- aminopropyl vinyl ethers, 2- ammonia
One or more of base butyl vinyl ether is with the mixed mixture of arbitrary ratio.
The initiator is that one or more of ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate are mixed with arbitrary ratio
Mixture.
A kind of preparation method of research of non-phosphorus scale inhibitor, is achieved by the steps of：
(1) cyclodextrin, the vinyl ethers with amino, water are added into stirring-type polymer reactor, opens stirring, and
Begin to warm up heating；
(2) when the temperature in stirring-type polymer reactor rises to 105 DEG C~135 DEG C, start be added dropwise mass concentration be 1~
7% initiator solution, this initiator solution are formulated by the initiator and water, and time for adding was controlled at 3~6 hours；
(3) after dripping, then epoxychloropropane is added in stirring-type polymer reactor, keeping temperature, the reaction was continued 1~3
Hour, cooling discharge is to get the research of non-phosphorus scale inhibitor.
The cyclodextrin is that one or more of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin are mixed with arbitrary ratio
The mixture of conjunction.
The vinyl ethers with amino are 2- amino-ethyls vinyl ethers, 3- aminopropyl vinyl ethers, 2- ammonia
One or more of base butyl vinyl ether is with the mixed mixture of arbitrary ratio.
The initiator is that one or more of ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate are mixed with arbitrary ratio
Mixture.
Compared with prior art, the present invention has following remarkable result：
1. product of the present invention is nontoxic, pollution-free, not only dirty particle can also be removed into scale inhibition, reach scale inhibition even
The purpose of scale removal.
2. product of the present invention is not phosphorous, phosphorus-containing wastewater discharge is directly avoided to cause Water Eutrophication problem.
3. product of the present invention contains the various actives such as ether, hydroxyl and amino functional group, product of the present invention is by these functions
Group is integrated in one, and utilizes the synergistic effect between them so that it has better scale inhibition, dispersion performance.
The simple production process of product of the present invention, raw materials for production are easy to get, with short production cycle, and reaction is mild, and required equipment is
Conventional equipment is convenient for industrialized production.
Specific implementation mode
The present invention is further elaborated on reference to embodiments.
A kind of research of non-phosphorus scale inhibitor of the present invention, the raw material components matched by following mass fractions are made：
The cyclodextrin is that one or more of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin are mixed with arbitrary ratio
The mixture of conjunction.
The vinyl ethers with amino are 2- amino-ethyls vinyl ethers, 3- aminopropyl vinyl ethers, 2- ammonia
One or more of base butyl vinyl ether is with the mixed mixture of arbitrary ratio.
The initiator is that one or more of ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate are mixed with arbitrary ratio
Mixture.
A kind of preparation method of research of non-phosphorus scale inhibitor of the present invention, is achieved by the steps of：
(1) cyclodextrin, the vinyl ethers with amino, water are added into stirring-type polymer reactor, opens stirring, and
Begin to warm up heating；
(2) when the temperature in stirring-type polymer reactor rises to 105 DEG C~135 DEG C, start be added dropwise mass concentration be 1~
7% initiator solution, this initiator solution are formulated by the initiator and water, and time for adding was controlled at 3~6 hours；
(3) after dripping, then epoxychloropropane is added in stirring-type polymer reactor, keeping temperature, the reaction was continued 1~3
Hour, cooling discharge is to get the research of non-phosphorus scale inhibitor.
With specific embodiment, the present invention is described in detail below, but the present invention is not limited only to this.
Embodiment 1
A kind of research of non-phosphorus scale inhibitor of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of research of non-phosphorus scale inhibitor of the present invention, is achieved by the steps of：
(1) 31 parts of alpha-cyclodextrins, 1.5 parts of 2- amino-ethyls vinyl ethers, 61.3 are added into stirring-type polymer reactor
Part water, opens stirring, and begin to warm up heating；
(2) when the temperature in stirring-type polymer reactor rises to 108 DEG C, it is 1.6% to draw to start to be added dropwise mass concentration
Agent solution is sent out, this initiator solution is formulated by 0.08 part of ammonium persulfate and 4.92 parts of water, and time for adding control is small 3.5
When；
(3) after dripping, then 1.2 parts of epoxychloropropane are added in stirring-type polymer reactor, keep temperature to continue anti-
It answers 1.2 hours, cooling discharge is to get the research of non-phosphorus scale inhibitor.
Embodiment 2
A kind of research of non-phosphorus scale inhibitor of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of research of non-phosphorus scale inhibitor of the present invention, is achieved by the steps of：
(1) add 32.7 parts into stirring-type polymer reactor and enter alpha-cyclodextrin, 2.8 parts of 2- amino-ethyls vinyl ethers, 53
Part water, opens stirring, and begin to warm up heating；
(2) when the temperature in stirring-type polymer reactor rises to 116 DEG C, it is 1.3% to draw to start to be added dropwise mass concentration
Agent solution is sent out, this initiator solution is formulated by 0.13 part of ammonium persulfate and 9.87 parts of water, and time for adding control is small 4.1
When；
(3) after dripping, then 1.5 parts of epoxychloropropane are added in stirring-type polymer reactor, keep temperature to continue anti-
It answers 2.2 hours, cooling discharge is to get the research of non-phosphorus scale inhibitor.
Embodiment 3
A kind of research of non-phosphorus scale inhibitor of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of research of non-phosphorus scale inhibitor of the present invention, is achieved by the steps of：
(1) into stirring-type polymer reactor be added 34.2 parts of beta-cyclodextrins, 4.2 parts of 3- aminopropyl vinyl ethers,
49.3 parts of water open stirring, and begin to warm up heating；
(2) when the temperature in stirring-type polymer reactor rises to 121 DEG C, it is 2.8% to draw to start to be added dropwise mass concentration
Agent solution is sent out, this initiator solution is formulated by 0.28 part of sodium peroxydisulfate and 9.72 parts of water, and time for adding control is small 4.6
When；
(3) after dripping, then 2.3 parts of epoxychloropropane are added in stirring-type polymer reactor, keep temperature to continue anti-
It answers 2.8 hours, cooling discharge is to get the research of non-phosphorus scale inhibitor.
Embodiment 4
A kind of research of non-phosphorus scale inhibitor of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of research of non-phosphorus scale inhibitor of the present invention, is achieved by the steps of：
(1) into stirring-type polymer reactor be added 36.5 parts of beta-cyclodextrins, 6.7 parts of 3- aminopropyl vinyl ethers,
43.3 parts of water open stirring, and begin to warm up heating；
(2) when the temperature in stirring-type polymer reactor rises to 128 DEG C, it is 4.5% to draw to start to be added dropwise mass concentration
Agent solution is sent out, this initiator solution is formulated by 0.45 part of sodium peroxydisulfate and 9.55 parts of water, and time for adding control is small 5.7
When；
(3) after dripping, then 3.5 parts of epoxychloropropane are added in stirring-type polymer reactor, keep temperature to continue anti-
It answers 1.6 hours, cooling discharge is to get the research of non-phosphorus scale inhibitor.
Embodiment 5
A kind of research of non-phosphorus scale inhibitor of the present invention, the raw material components matched by following mass fractions are made：
A kind of preparation method of research of non-phosphorus scale inhibitor of the present invention, is achieved by the steps of：
(1) into stirring-type polymer reactor be added 38.3 parts of gamma-cyclodextrins, 8.5 parts of 2- aminobutyls vinyl ethers,
39.1 parts of water open stirring, and begin to warm up heating；
(2) when the temperature in stirring-type polymer reactor rises to 125 DEG C, it is 6.1% to draw to start to be added dropwise mass concentration
Agent solution is sent out, this initiator solution is formulated by 0.61 part of potassium peroxydisulfate and 9.39 parts of water, and time for adding control is small 5.5
When；
(3) after dripping, then 4.1 parts of epoxychloropropane are added in stirring-type polymer reactor, keep temperature to continue anti-
It answers 2.9 hours, cooling discharge is to get the research of non-phosphorus scale inhibitor.
Embodiment 6
A kind of research of non-phosphorus scale inhibitor of the present invention, the raw material components matched by following mass fractions are made：
Wherein, the vinyl ethers with amino are using 2- amino-ethyls vinyl ethers and 3- aminopropyl vinyl ethers
Mixture, and the mass ratio of 2- amino-ethyls vinyl ethers and 3- aminopropyl vinyl ethers is 15:16, that is, 2- amino-ethyls
The dosage of vinyl ethers and 3- aminopropyl vinyl ethers is respectively 4.5 parts and 4.8 parts.
Initiator uses the mixture of ammonium persulfate and sodium peroxydisulfate, and the mass ratio of ammonium persulfate and sodium peroxydisulfate is 1:
2, that is, the dosage of ammonium persulfate and sodium peroxydisulfate is respectively 0.22 part and 0.44 part.
A kind of preparation method of research of non-phosphorus scale inhibitor of the present invention, is achieved by the steps of：
(1) into stirring-type polymer reactor be added 39.1 parts of gamma-cyclodextrins, 4.5 parts of 2- amino-ethyls vinyl ethers,
4.8 parts of 3- aminopropyl vinyl ethers, 36.7 parts of water open stirring, and begin to warm up heating；
(2) when the temperature in stirring-type polymer reactor rises to 131 DEG C, it is 6.6% to draw to start to be added dropwise mass concentration
Agent solution is sent out, this initiator solution is formulated by 0.22 part of ammonium persulfate, 0.44 part of sodium peroxydisulfate and 9.34 parts of water, when dropwise addition
Between control at 5 hours；
(3) after dripping, then 4.9 parts of epoxychloropropane are added in stirring-type polymer reactor, keep temperature to continue anti-
It answers 2.2 hours, cooling discharge is to get the research of non-phosphorus scale inhibitor.
It is to carry out contrast test with commercially available organophosphor antisludging agent using the antisludging agent of the present invention below, illustrates its effect
Fruit.
Table 1 tests water quality index
| Project | Index |
| PH value | 9.32 |
| SS/(mg·L-1) | 65 |
| Total alkalinity/(with CaCO3Count mgL-1) | 2200 |
| Calcium hardness/(with CaCO3Count mgL-1) | 500 |
| Total hardness/(with CaCO3Count mgL-1) | 650 |
| Chlorion/(mgL-1) | 400 |
| Conductivity/(uscm-1) | 4000 |
GB/T16632-2008 " measurement of water treatment agent scale-inhibiting properties " evaluates the performance of antisludging agent according to national standards, this
Product is shown in Table 2 with commercially available organophosphor performance of antisludging agent comparing result.
Product prepared by 2 embodiment of the present invention 1~6 of table is compared with commercially available organophosphor performance of antisludging agent
As known from Table 2, the antisludging agent product that prepared by the embodiment of the present invention 1~6, is significantly better than that commercially available organic in performance
Phosphorus antisludging agent, and handle and do not contain phosphate anion in water, avoid pollution of the phosphate radical to water body.
The method of the present invention is described by specific embodiment.Those skilled in the art can use for reference this hair
The links such as the appropriate feed change of bright content, process conditions realize corresponding other purposes, correlation change all without departing from
Present disclosure, all similar substitutions and modifications are it will become apparent to those skilled in the art that be considered as
It is included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of research of non-phosphorus scale inhibitor, it is characterised in that：It is achieved by the steps of：
(1) cyclodextrin, the vinyl ethers with amino, water are added into stirring-type polymer reactor, opens stirring, and start
Heat temperature raising；
(2) when the temperature in stirring-type polymer reactor rises to 105 DEG C~135 DEG C, start that mass concentration is added dropwise to be 1~7%
Initiator solution, this initiator solution is formulated by the initiator and water, and time for adding was controlled at 3~6 hours；
(3) after dripping, then epoxychloropropane is added in stirring-type polymer reactor, keeps temperature the reaction was continued 1~3 small
When, cooling discharge is to get the research of non-phosphorus scale inhibitor.
2. research of non-phosphorus scale inhibitor according to claim 1, it is characterised in that：The raw material components system matched by following mass fractions
At：
3. research of non-phosphorus scale inhibitor according to claim 2, it is characterised in that：The cyclodextrin is alpha-cyclodextrin, beta-cyclodextrin
With one or more of gamma-cyclodextrin with the mixed mixture of arbitrary ratio.
4. research of non-phosphorus scale inhibitor according to claim 2, it is characterised in that：The vinyl ethers with amino are 2- ammonia
One or more of base ethyl vinyl ether, 3- aminopropyl vinyl ethers, 2- aminobutyl vinyl ethers are with arbitrary
Than mixed mixture.
5. research of non-phosphorus scale inhibitor according to claim 2, it is characterised in that：The initiator is ammonium persulfate, sodium peroxydisulfate
With one or more of potassium peroxydisulfate with the mixed mixture of arbitrary ratio.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810790338.XA CN108706751A (en) | 2018-07-18 | 2018-07-18 | A kind of research of non-phosphorus scale inhibitor and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810790338.XA CN108706751A (en) | 2018-07-18 | 2018-07-18 | A kind of research of non-phosphorus scale inhibitor and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145256A (en) * | 2013-03-18 | 2013-06-12 | 武汉理工大学 | Preparation method and application of ternary high polymer copolymer scale inhibitor |
| CN104556428A (en) * | 2013-10-14 | 2015-04-29 | 中国石油化工股份有限公司 | Composition for corrosion inhibition and scale inhibition and application of composition |
| CN108002554A (en) * | 2017-11-09 | 2018-05-08 | 王林双 | The preparation method and slow-release scale inhibitor of a kind of slow-release scale inhibitor |
-
2018
- 2018-07-18 CN CN201810790338.XA patent/CN108706751A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145256A (en) * | 2013-03-18 | 2013-06-12 | 武汉理工大学 | Preparation method and application of ternary high polymer copolymer scale inhibitor |
| CN104556428A (en) * | 2013-10-14 | 2015-04-29 | 中国石油化工股份有限公司 | Composition for corrosion inhibition and scale inhibition and application of composition |
| CN108002554A (en) * | 2017-11-09 | 2018-05-08 | 王林双 | The preparation method and slow-release scale inhibitor of a kind of slow-release scale inhibitor |
Non-Patent Citations (2)
| Title |
|---|
| 刘圆: "环糊精基团对氧乙烯醚结构和性能的作用", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 赵朝锋: "环糊精及其聚合物的结构、性质及应用", 《矿业科学技术》 * |
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