CN104909440A - New composite ethyl orthosilicate-polyaluminium chloride flocculant preparation method - Google Patents
New composite ethyl orthosilicate-polyaluminium chloride flocculant preparation method Download PDFInfo
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- CN104909440A CN104909440A CN201510213127.6A CN201510213127A CN104909440A CN 104909440 A CN104909440 A CN 104909440A CN 201510213127 A CN201510213127 A CN 201510213127A CN 104909440 A CN104909440 A CN 104909440A
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Abstract
The invention discloses a new composite ethyl orthosilicate-polyaluminium chloride flocculant preparation method. Through high temperature curing processing of traditional polyaluminium chloride, higher content of aluminum 30 form can be obtained, during curing, ethyl orthosilicate is introduced, and a new composite ethyl orthosilicate-polyaluminium chloride flocculant product is synthesized; the new composite ethyl orthosilicate-polyaluminium chloride flocculant product contains high content of nano aluminum 30 and silicon sol, can play efficient electricity neutralization capability of the aluminum 30, and can play the adsorption bridge enhancement capacity of the silicon sol, better effect of coagulation can be achieved, the use range of the flocculant can be broadened, and the problems of not good flocculation effect and narrow feed dose range of the traditional polyaluminium chloride flocculant can be solved.
Description
Technical field
The invention belongs to drinking water safety guarantee and all kinds of sewage treatment area, be specifically related to the preparation method of a kind of NEW TYPE OF COMPOSITE tetraethoxy-flocculant of polymeric aluminium chloride.
Background technology
In current water-treatment technology field, inorganic polymer flocculant is the special chemical agent that usage quantity is very large.Compared with traditional flocculant, it can significantly improve purification efficiency, and have low-consuming, settling property good, security is high, adapt to the advantages such as wide, therefore at home and abroad water treatment field is used widely and is developed rapidly.Wherein, polymerize aluminum chloride (PAC) is that current industrial production technology is the most ripe, usefulness is the highest, applies also inorganic polymer flocculant kind the most widely.It is generally acknowledged, aluminium 13 (Al13) form carrying capacity in polymerize aluminum chloride is high, and charge neutrality ability is strong, also has stronger adsorption bridging ability, be the best cohesion flocculation morphology in flocculant of polymeric aluminium chloride, how much its content reflects the flocculation performance of goods.Recently the research of polymeric aluminum is shown again, aluminium 30 (Al30) is also a kind of advantage coagulation form, relative to aluminium 13, there is higher carrying capacity and larger space scale, but because its content in traditional polymerize aluminum chloride product is extremely low, more difficultly to play a role, therefore how to improve the target that Al30 form content in polymerize aluminum chloride becomes coagulating agent development from now on.
Recent two decades comes, and in order to adapt to, water treatment field is safer to inorganic polymer coagulant, needs efficiently, expands the development work of various efficient flocculant both at home and abroad.Wherein study more be the method such as compound, copolymerization for inorganic polymer flocculant.In order to increase the adsorption bridging ability of inorganic polymer coagulant, also do the work such as inorganic-organic hybrid, graft modification, also some effects are achieved, such as organosilicon-aluminium compound (composite) coagulating agent, the product made by wishing can play the synergy of various active principle.Wherein organosilicon directly can obtain and be hydrolyzed rear usual with activated silica solation performance Coagulation aiding, therefore, both aluminium 30 and organosilicon is combined and has market outlook very much with the coagulating agent development work of collaborative charge neutrality and bridging action.
Summary of the invention
Goal of the invention: in order to solve the deficiencies in the prior art, the invention provides the preparation method of a kind of NEW TYPE OF COMPOSITE tetraethoxy-flocculant of polymeric aluminium chloride, this product contains nano aluminum 30 and the silicon sol of high level, the efficient electric neutralising capacity of aluminium 30 can be played, silicon sol can be played again and strengthen adsorption bridging ability, thus reach better coagulation effect, widen the use range of this flocculation agent.
Technical scheme 1: a kind of preparation method of NEW TYPE OF COMPOSITE tetraethoxy-flocculant of polymeric aluminium chloride, comprises the steps:
(1) preparation of polymeric aluminum chlorides solution:
Adopt and slowly add alkali paddling process: the AlCl measuring the 0.5mol/L of predetermined amount
3solution, under intense agitation, slowly adds with peristaltic pump the NaOH solution that concentration is 0.5mol/L, the amount of required alkali lye is determined according to predetermined basicity, add alkali speed and be about 0.15ml/min, continue stirring after alkali lye all adds 2 hours, be placed in 4 DEG C of preservations in refrigerator;
(2) high-temperature maturing process:
In closed reactor, high-temperature maturing is carried out to polymerize aluminum chloride, temperature is 90 DEG C ~ 100 DEG C, slaking is after 48 hours, add a certain amount of tetraethoxy, the mol ratio of silicon and aluminium in polysilicate aluminum chloride is made to be 0.01-0.1, continue high-temperature maturing 2 hours, want Keep agitation in the process, material is fully mixed;
(3) cool:
Carried out naturally cooling to room temperature by above-mentioned obtained product, obtain final finished, wherein, aluminium 30 content is about 30%, and the mol ratio of silicon and aluminium is 0.01-0.1.
Technical scheme 2:
The preparation method of another kind of NEW TYPE OF COMPOSITE tetraethoxy-flocculant of polymeric aluminium chloride, adopts following steps:
A () first prepares polymerization tetraethoxy-polymeric aluminum chlorides solution:
Adopt and slowly add alkali paddling process: the ratio being first 0.01-0.1 in silica alumina ratio is added tetraethoxy and jointly reacted obtained compound tetraethoxy-polymeric aluminum chlorides solution, the total aluminium concentration of described polymerization tetraethoxy-liquor alumini chloridi is 0.2M, basicity is 2.4, and silica alumina ratio is 0.01-0.1;
The process of (b) high-temperature maturing:
In closed reactor, carry out high-temperature maturing to this polymerization tetraethoxy-liquor alumini chloridi, it is 90 DEG C that temperature controls, and slaking is after 24 hours, and continue insulation 12 hours, maturing process Keep agitation makes material fully mix, and the overall curing time is 36 hours;
C () cools:
Carried out naturally cooling to room temperature by above-mentioned obtained product, obtain final finished, wherein, aluminium 30 content is about 30%, and the mol ratio of silicon and aluminium is 0.01-0.1.
Beneficial effect: the present invention carries out high-temperature maturing process to conventional polymeric aluminum chloride, obtain aluminium 30 form of high level, between the maturation period, introduce tetraethoxy in good time, thus synthesize a kind of novel flocculant product of compound tetraethoxy-polymerize aluminum chloride.This product contains nano aluminum 30 and the silicon sol of high level, can play the efficient electric neutralising capacity of aluminium 30, can play again silicon sol and strengthen adsorption bridging ability, thus reach better coagulation effect, widen the use range of this flocculation agent.Solve conventional polymeric aluminum chloride flocculant flocculating effect not good, throw in the problem that dosage range is narrower.
Preparation process is carried out in closed reactor, temperature at 90 ~ 100 DEG C, can before slaking in after add the tetraethoxy of certain silica alumina ratio, ensure in adding procedure that Keep agitation makes material fully mix, the overall curing time is 10 ~ 50 hours, and last room temperature cooling obtains product.
Product total aluminium concentration can be mixed with 0.2M, basicity 2.4, and wherein aluminium 30 content is about 30%, and silica alumina ratio is between 0.01-0.1.
This product obviously can widen effective dosage scope.Traditional 0.2M, the polymerize aluminum chloride of basicity 2.4 be 70 to turbidity, UV
254be 0.6, in 30 minutes coagulation experiments of the kaolin-humic acid suspension liquid system of pH9.0, temperature 20 DEG C, effective dosage scope is between 0.1-0.425mmol/L; And effective dosage scope that this product is removed turbidity is between 0.05-0.75mmol/L, significantly broadens, and most high concentrtion clearance rate and UV
254clearance rate can up to 99% and 70%.
Embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail.
Specific embodiment one:
(1) preparation of polymeric aluminum chlorides solution:
Adopt and slowly add alkali paddling process to obtain total aluminium concentration be 0.2M, basicity is the polymeric aluminum chlorides solution of 2.4.
(2) high-temperature maturing process:
In closed reactor, high-temperature maturing is carried out to obtained polymerize aluminum chloride, temperature is 90 DEG C, slaking is after 48 hours, add a certain amount of tetraethoxy, the mol ratio of silicon and aluminium in polysilicate aluminum chloride is made to be 0.01, continue high-temperature maturing 2 hours, want Keep agitation in the process, material is fully mixed.
(3) cool:
Carried out naturally cooling to room temperature by above-mentioned obtained product, obtain final finished, wherein, aluminium 30 content is 40%, and the mol ratio of silicon and aluminium is 0.01.
Specific embodiment two:
(1) preparation of polymeric aluminum chlorides solution:
Adopt and slowly add alkali paddling process to obtain total aluminium concentration be 0.2M, basicity is the polymeric aluminum chlorides solution of 2.4.
(2) high-temperature maturing process:
In closed reactor, carry out high-temperature maturing to polymerize aluminum chloride, temperature is 90 DEG C, and slaking is after 48 hours, add a certain amount of tetraethoxy, make the mol ratio of silicon and aluminium in polysilicate aluminum chloride be 0.05, continue high-temperature maturing 2 hours, want Keep agitation in the process, material is fully mixed.
(3) cool:
Carried out naturally cooling to room temperature by above-mentioned obtained product, obtain final finished, wherein, aluminium 30 content is 30%, and the mol ratio of silicon and aluminium is 0.05.
Specific embodiment three:
A preparation method for NEW TYPE OF COMPOSITE tetraethoxy aluminum chloride flocculant, comprises the steps:
(1) preparation of polymeric aluminum chlorides solution:
Adopt and slowly add alkali paddling process to obtain total aluminium concentration be 0.2M, basicity is the polymeric aluminum chlorides solution of 2.4.
(2) high-temperature maturing process:
In closed reactor, carry out high-temperature maturing to polymerize aluminum chloride, temperature is 90 DEG C, and slaking is after 48 hours, add a certain amount of tetraethoxy, make the mol ratio of silicon and aluminium in polysilicate aluminum chloride be 0.1, continue high-temperature maturing 2 hours, want Keep agitation in the process, material is fully mixed;
(3) cool:
Carried out naturally cooling to room temperature by above-mentioned obtained product, obtain final finished, wherein, aluminium 30 content is 25%, and the mol ratio of silicon and aluminium is 0.1.
Specific embodiment four:
The preparation method of another kind of NEW TYPE OF COMPOSITE tetraethoxy aluminum chloride flocculant, adopts following steps:
A () first prepares polymerization tetraethoxy-liquor alumini chloridi:
Adopt and slowly add alkali paddling process: the ratio being first 0.1 in silica alumina ratio is added tetraethoxy and jointly reacted obtained polymerization tetraethoxy-liquor alumini chloridi, the total aluminium concentration of described polymerization tetraethoxy-liquor alumini chloridi is 0.2M, basicity is 2.4, and silica alumina ratio is 0.1;
The process of (b) high-temperature maturing:
Then in closed reactor, carry out high-temperature maturing to this polymerization tetraethoxy-liquor alumini chloridi, it is 90 DEG C that temperature controls, and slaking is after 24 hours, continue insulation 12 hours, maturing process Keep agitation makes material fully mix, and the overall curing time is 36 hours, naturally cooling;
C () cools:
Carried out naturally cooling to room temperature by above-mentioned obtained product, obtain final finished, wherein, aluminium 30 content is 45%, and the mol ratio of silicon and aluminium is 0.1.
The present invention is not limited to above-mentioned preferred forms; anyone can draw other various forms of products under enlightenment of the present invention; no matter but any change is done in its shape or structure; every have identical with the application or akin technical scheme, all drops within protection scope of the present invention.
Claims (5)
1. a preparation method for NEW TYPE OF COMPOSITE tetraethoxy-flocculant of polymeric aluminium chloride, is characterized in that: comprise the steps:
(1) preparation of polymeric aluminum chlorides solution:
Adopt and slowly add alkali paddling process: the AlCl measuring the 0.5mol/L of predetermined amount
3solution, under intense agitation, slowly adds with peristaltic pump the NaOH solution that concentration is 0.5mol/L, the amount of required alkali lye is determined according to predetermined basicity, add alkali speed and be about 0.15ml/min, continue stirring after alkali lye all adds 2 hours, be placed in 4 DEG C of preservations in refrigerator;
(2) high-temperature maturing process:
In closed reactor, high-temperature maturing is carried out to polymerize aluminum chloride, temperature is 90 DEG C ~ 100 DEG C, slaking is after 48 hours, add a certain amount of tetraethoxy, the mol ratio of silicon and aluminium in polysilicate aluminum chloride is made to be 0.01-0.1, continue high-temperature maturing 2 hours, want Keep agitation in the process, material is fully mixed;
(3) cool:
Carried out naturally cooling to room temperature by above-mentioned obtained product, obtain final finished, wherein, aluminium 30 content is about 30%, and the mol ratio of silicon and aluminium is 0.01-0.1.
2. the preparation method of NEW TYPE OF COMPOSITE tetraethoxy-flocculant of polymeric aluminium chloride according to claim 1, it is characterized in that: in described step (1), the total aluminium concentration of obtained polymeric aluminum chlorides solution is 0.2M, basicity is 2.4, in described step (2), pyrolytic conversion temperature is at 90-100 DEG C, and transformation time is 10-50 hour, and silica alumina ratio is between 0.01-0.1.
3. a preparation method for NEW TYPE OF COMPOSITE tetraethoxy-flocculant of polymeric aluminium chloride, is characterized in that: adopt following steps:
A () first prepares polymerization tetraethoxy-polymeric aluminum chlorides solution:
Adopt and slowly add alkali paddling process: the ratio being first 0.01-0.1 in silica alumina ratio is added tetraethoxy and jointly reacted obtained compound tetraethoxy-polymeric aluminum chlorides solution, the total aluminium concentration of described polymerization tetraethoxy-liquor alumini chloridi is 0.2M, basicity is 2.4, and silica alumina ratio is 0.01-0.1;
The process of (b) high-temperature maturing:
In closed reactor, carry out high-temperature maturing to this polymerization tetraethoxy-liquor alumini chloridi, it is 90 DEG C that temperature controls, and slaking is after 24 hours, and continue insulation 12 hours, maturing process Keep agitation makes material fully mix, and the overall curing time is 36 hours;
C () cools:
Carried out naturally cooling to room temperature by above-mentioned obtained product, obtain final finished, wherein, aluminium 30 content is about 30%, and the mol ratio of silicon and aluminium is 0.01-0.1.
4. the preparation method of NEW TYPE OF COMPOSITE tetraethoxy-flocculant of polymeric aluminium chloride according to claim 3, is characterized in that: be first compounded to form tetraethoxy-polymerize aluminum chloride, subsequently high-temperature maturing together.
5. compound tetraethoxy-flocculant of polymeric aluminium chloride that according to claim 1 or 3 prepared by method, is characterized in that: be 70 to turbidity, UV
254be 0.6, in 30 minutes coagulation experiments of the kaolin-humic acid suspension liquid system of pH9.0, temperature 20 DEG C, most high concentrtion clearance rate and UV
254clearance rate, respectively up to 99% and 70%, effectively throws in dosage range at 0.05-0.75mmol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111439865A (en) * | 2020-04-07 | 2020-07-24 | 中国科学院生态环境研究中心 | Defluorination method for coal gas wastewater |
| CN114772937A (en) * | 2021-11-11 | 2022-07-22 | 河源旗滨硅业有限公司 | Glass powder slurry treatment process |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911827A (en) * | 2006-09-07 | 2007-02-14 | 中国科学院生态环境研究中心 | Preparation of nanometer type inorganic polymer flocculant and its product |
| CN1915830A (en) * | 2006-09-07 | 2007-02-21 | 中国科学院生态环境研究中心 | Method for purifying Al13 in high yield |
| JP2007167721A (en) * | 2005-12-20 | 2007-07-05 | Taki Chem Co Ltd | Flocculant for wastewater treatment |
| CN102092827A (en) * | 2010-12-01 | 2011-06-15 | 清华大学 | Composite polyaluminum silicate chloride and preparation method thereof |
| CN103130258A (en) * | 2011-11-28 | 2013-06-05 | 中国科学院生态环境研究中心 | Preparation method of polymeric aluminum with high concentration high alcohol (Alc) content by making use of membrane distillation technology |
| CN104056594A (en) * | 2013-12-25 | 2014-09-24 | 南通大学 | Clay mineral absorbing material applied to water treatment and preparation method thereof |
| CN104478051A (en) * | 2014-12-10 | 2015-04-01 | 上海应用技术学院 | Method for preparing poly-aluminum ferric silicate sulfate flocculating agent |
-
2015
- 2015-04-29 CN CN201510213127.6A patent/CN104909440A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007167721A (en) * | 2005-12-20 | 2007-07-05 | Taki Chem Co Ltd | Flocculant for wastewater treatment |
| CN1911827A (en) * | 2006-09-07 | 2007-02-14 | 中国科学院生态环境研究中心 | Preparation of nanometer type inorganic polymer flocculant and its product |
| CN1915830A (en) * | 2006-09-07 | 2007-02-21 | 中国科学院生态环境研究中心 | Method for purifying Al13 in high yield |
| CN102092827A (en) * | 2010-12-01 | 2011-06-15 | 清华大学 | Composite polyaluminum silicate chloride and preparation method thereof |
| CN103130258A (en) * | 2011-11-28 | 2013-06-05 | 中国科学院生态环境研究中心 | Preparation method of polymeric aluminum with high concentration high alcohol (Alc) content by making use of membrane distillation technology |
| CN104056594A (en) * | 2013-12-25 | 2014-09-24 | 南通大学 | Clay mineral absorbing material applied to water treatment and preparation method thereof |
| CN104478051A (en) * | 2014-12-10 | 2015-04-01 | 上海应用技术学院 | Method for preparing poly-aluminum ferric silicate sulfate flocculating agent |
Non-Patent Citations (3)
| Title |
|---|
| 叶长青，等: "复合聚硅铝三十絮凝剂的混凝性能研究", 《环境科学与技术》 * |
| 赵奎霞，等: "聚硅氯化铝絮凝剂的中聚合态特征", 《中国矿业大学学报》 * |
| 高宝玉，等: "聚硅氯化铝(PASC)混凝剂的颗粒大小及分子量分布", 《中国环境科学》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111439865A (en) * | 2020-04-07 | 2020-07-24 | 中国科学院生态环境研究中心 | Defluorination method for coal gas wastewater |
| CN111439865B (en) * | 2020-04-07 | 2022-02-25 | 中国科学院生态环境研究中心 | Defluorination method for coal gas wastewater |
| CN114772937A (en) * | 2021-11-11 | 2022-07-22 | 河源旗滨硅业有限公司 | Glass powder slurry treatment process |
| CN114772937B (en) * | 2021-11-11 | 2023-12-19 | 河源旗滨硅业有限公司 | Glass powder slurry treatment process |
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