CN103979655B - A kind of sewage treatment drug and preparation method thereof - Google Patents
A kind of sewage treatment drug and preparation method thereof Download PDFInfo
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- CN103979655B CN103979655B CN201310530607.6A CN201310530607A CN103979655B CN 103979655 B CN103979655 B CN 103979655B CN 201310530607 A CN201310530607 A CN 201310530607A CN 103979655 B CN103979655 B CN 103979655B
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- solution
- tio
- sewage treatment
- aluminum chloride
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of sewage treatment drug and preparation method thereof, it is characterized in that this sewage treatment drug is composited by titanium dioxide and polymerize aluminum chloride; The preparation method of this medicament comprises the following steps: first, in hydrochloric acid (HCl), adds aluminum chloride (AlCl
3) solid, be stirred to aluminum chloride and all dissolve, obtain solution A; Secondly, in concentrated hydrochloric acid, organic titanate is added---butyl (tetra) titanate (Ti (OC
4h
9)
4), be stirred to and present transparent clarification shape, obtain solution B; Subsequently, solution A and solution B are transferred in hydrothermal reaction kettle, control temperature of reaction and time, obtain solution C; Then, evaporating solns C obtains containing crystalline A lCl
3with titanium dioxide (TiO
2) mixture, by product propyl carbinol and HCl gas absorb obtained dilute hydrochloric acid by water, and propyl carbinol recycles as dispersion agent; Finally, crystalline A lCl
3and TiO
2, add water, be hydrolyzed at a certain temperature, preparation is containing TiO
2polymerize aluminum chloride.The present invention TiO that adopted chemical process to prepare
2compound sewage treatment agent with polymerize aluminum chloride, has flocculating effect good, and sedimentation is fast, reduces the function of COD.
Description
Technical field
The present invention relates to technical field of sewage, particularly a kind of preparation method of sewage treatment drug.
Background technology
Along with the raising of industrialization, the level of urbanization, the discharge of a large amount of industrial sewage, sanitary sewage creates pollution to water body, destroys ecology, the production of serious harm industrial or agricultural and HUMAN HEALTH.The pollutent difficult containing all kinds of biochemical degradation in the water inlet of current domestic sewage work, colourity is high, COD is high, need to consume a large amount of sewage treatment drugs, especially widely used a kind of flocculation agent---poly aluminium chloride in sewage disposal, its low price, functional, but this material also has some defects, such as alumen ustum is little, settling velocity is slow, performance is single, therefore selects efficient sewage treatment drug to become a kind of active demand.
Titanic oxide material (TiO
2) be a kind of very important semiconductor material, there is excellent physics, chemical property, this material mainly contains 3 kinds of crystal formations, i.e. anatase octahedrite, rutile and brookite, this material has plurality of advantages, as low price, safety, stable, nontoxic, pollution-free etc., be widely used in the fields such as paint, coating, chemical fibre, pottery, especially playing an important role in photocatalysis to degrade organic matter field.
CN 101595066A reports water purification composition, comprises condensing agent, flocculation agent, sorbent material and biocides, using polymerize aluminum chloride as flocculation agent, and TiO
2as sorbent material, effectively reduce the arsenic in water; CN 101362621A reports a kind of technology processing native rubber processing waste water, adopts UV/ nano-TiO
2, effectively removes ammonia nitrogen and COD.These two patents all indicate TiO
2critical function in sewage disposal, but all belong to physics interpolation, do not relate to chemically composited.
Chemical method is the important method that a kind of synthesis has ordered structure, premium properties, multicomponent composite materials, have equipment simple, operate the plurality of advantages such as simple and easy, with low cost.
Summary of the invention
The object of the present invention is to provide a kind of sewage treatment drug and preparation method thereof, make this medicament have flocculating effect good, sedimentation is fast, reduces the function of COD.
The technical solution realizing the object of the invention is: concrete steps are as follows: first, in hydrochloric acid (HCl), adds aluminum chloride (AlCl
3) solid, be stirred to aluminum chloride and all dissolve, obtain solution A; Secondly, in concentrated hydrochloric acid, butyl (tetra) titanate (Ti (OC is added
4h
9)
4), be stirred to and present transparent clarification shape, obtain solution B; Subsequently, solution A and solution B are transferred in hydrothermal reaction kettle, control temperature of reaction and time, obtain solution C; Then, evaporating solns C obtains containing crystalline A lCl
3with titanium dioxide (TiO
2) mixture, by product propyl carbinol and HCl gas absorb obtained dilute hydrochloric acid by water, and propyl carbinol recycles as dispersion agent; Finally, crystalline A lCl
3and TiO
2, add water, be hydrolyzed at a certain temperature, preparation is containing TiO
2polymerize aluminum chloride.
Wherein, AlCl is dissolved in solution A
3concentration of hydrochloric acid controls as 10-20%;
Wherein, Ti (OC in solution B
4h
9)
4be dissolved in 37% concentrated hydrochloric acid, Ti (OC
4h
9)
4with hydrochloric acid mol ratio control 1:4-1:8, Ti (OC
4h
9)
4with AlCl
3mol ratio span of control is 1:4-1:40, and by product propyl carbinol recycles as dispersion agent;
Wherein, solution A and the solution B reaction times in hydrothermal reaction kettle is 12h-48h, and temperature range controls 50
oc-100
oc;
Wherein, solution C evaporates boiling under condition of negative pressure, obtained crystalline A lCl
3and TiO
2mixture, boiling temperature control 140
oc-180
oc;
Wherein, by product propyl carbinol and HCl gas absorb through water, obtained dilute hydrochloric acid concentration range control 10%-20%;
Wherein, crystalline A lCl
3and TiO
2, hydrolysis temperature controls 60
oc-80
oc, pH control 3.5-5.5, time controling 2h-6h;
Wherein, TiO in polymerize aluminum chloride
2mass content control as 2%-20%.
The present invention compared with prior art, its remarkable advantage: one, with organic titanate for mixing agent, adopt chemical method prepared sewage treatment drug---containing TiO
2polymerize aluminum chloride; Two, this sewage treatment drug has the multi-functionals such as flocculation agent, sorbent material, degradation agents, discoloring agent; Three, in sewage disposal, the use of this medicament reduces the usage quantity of other medicament (as discoloring agent, degradation agents); Prepared by the compound that four, the method can be promoted for other sewage treatment drug.
Embodiment
Further illustrate technical solution of the present invention below in conjunction with specific embodiment, these embodiments can not be interpreted as the restriction to technical scheme.
Embodiment 1: prepare a kind of sewage treatment drug according to following concrete steps
Step 1, in 20mL10% hydrochloric acid (HCl), adds aluminum chloride (AlCl
3) solid 10g, mechanical stirring is all dissolved to aluminum chloride, obtains solution A;
Step 2, by 0.0075mol butyl (tetra) titanate (Ti (OC
4h
9)
4) drop in the dense HCl of 3.0g37%, violent stirring to solution presents transparent clarification shape, obtains solution B;
Step 3, pours into solution A and solution B in 50mL hydrothermal reaction kettle, temperature of reaction setting 50
oc, time controling 12h, is obtained by reacting solution C;
Step 4, under negative pressure (-0.2MPa) condition, evaporating solns C, evaporation boiling temperature controls 140
oc, obtained containing crystalline A lCl
3and TiO
2mixture, by product propyl carbinol and HCl gas absorb obtained dilute hydrochloric acid by water, and concentration is 10%;
Step 5, containing crystalline A lCl
3and TiO
2mixture, add 20mL water, hydrolysis temperature control 60
oc, pH control 3.5, time controling 2h, obtain containing TiO
2polymerize aluminum chloride.
Embodiment 2: prepare a kind of sewage treatment drug according to following concrete steps
Step 1, with embodiment 1;
Step 2, by 0.0075mol butyl (tetra) titanate (Ti (OC
4h
9)
4) drop in the dense HCl of 6.0g37%, violent stirring to solution presents transparent clarification shape, obtains solution B;
Step 3, with embodiment 1;
Step 4, with embodiment 1;
Step 5, with embodiment 1.
Embodiment 3: prepare a kind of sewage treatment drug according to following concrete steps
Step 1, with embodiment 1;
Step 2, with embodiment 1;
Step 3, pours into solution A and solution B in 50mL hydrothermal reaction kettle, temperature of reaction setting 100
oc, time controling 48h, is obtained by reacting solution C;
Step 4, with embodiment 1;
Step 5, with embodiment 1.
Embodiment 4: prepare a kind of sewage treatment drug according to following concrete steps
Step 1, with embodiment 1;
Step 2, with embodiment 1;
Step 3, with embodiment 1;
Step 4, under negative pressure (-0.1MPa) condition, evaporating solns C, evaporation boiling temperature controls 180
oc, obtained containing crystalline A lCl
3and TiO
2mixture, by product propyl carbinol and HCl gas absorb obtained dilute hydrochloric acid by water, and concentration is 20%;
Step 5, with embodiment 1.
Embodiment 5: prepare a kind of sewage treatment drug according to following concrete steps
Step 1, with embodiment 1;
Step 2, with embodiment 1;
Step 3, with embodiment 1;
Step 4, with embodiment 1;
Step 5, containing crystalline A lCl
3and TiO
2mixture, add 30mL water, hydrolysis temperature control 80
oc, pH control 5.5, time controling 6h, obtain containing TiO
2polymerize aluminum chloride.
Embodiment 6: prepare a kind of sewage treatment drug according to following concrete steps
Step 1, in 40mL20% hydrochloric acid (HCl), adds aluminum chloride (AlCl
3) solid 20g, mechanical stirring is all dissolved to aluminum chloride, obtains solution A;
Step 2, by 0.0188molTi (OC
4h
9)
4drop in the dense HCl of 14.8g37%, violent stirring to solution presents transparent clarification shape, obtains solution B;
Step 3, pours into solution A and solution B in 100mL hydrothermal reaction kettle, temperature of reaction setting 80
oc, time controling 24h, is obtained by reacting solution C;
Step 4, with embodiment 1;
Step 5, containing crystalline A lCl
3and TiO
2mixture, add 60mL water, hydrolysis temperature control 80
oc, pH control 4.0, time controling 4h, obtain containing TiO
2polymerize aluminum chloride.
Claims (5)
1. a preparation method for sewage treatment drug, comprises the following steps: first, in hydrochloric acid (HCl), adds aluminum chloride (AlCl
3) solid, be stirred to aluminum chloride and all dissolve, obtain solution A; Secondly, in concentrated hydrochloric acid, butyl (tetra) titanate (Ti (OC is added
4h
9)
4), be stirred to and present transparent clarification shape, obtain solution B; Subsequently, be transferred in hydrothermal reaction kettle by solution A and solution B, reaction times control 12h-48h, temperature range controls 50
oc-100
oc, obtains solution C; Then, under condition of negative pressure, evaporating solns C obtains containing crystalline A lCl
3with titanium dioxide (TiO
2) mixture, boiling temperature control 140
oc-180
oc, by product propyl carbinol and HCl gas absorb obtained dilute hydrochloric acid by water, and propyl carbinol recycles as dispersion agent; Finally, at crystalline A lCl
3and TiO
2in add water, hydrolysis temperature control 60
oc-80
oc, pH value control 3.5-5.5, time controling 2h-6h, preparation is containing TiO
2polymerize aluminum chloride.
2. the preparation method of a kind of sewage treatment drug according to claim 1, is characterized in that: dissolve AlCl in solution A
3concentration of hydrochloric acid controls as 10-20%.
3. the preparation method of a kind of sewage treatment drug according to claim 1, is characterized in that: Ti (OC in solution B
4h
9)
4be dissolved in 37% concentrated hydrochloric acid, Ti (OC
4h
9)
4with AlCl
3mol ratio span of control is 1:4-1:40.
4. the preparation method of a kind of sewage treatment drug according to claim 1, is characterized in that: HCl gas absorbs through water, obtains dilute hydrochloric acid concentration range control 10-20%, can be recycled in solution A.
5. the preparation method of a kind of sewage treatment drug according to claim 1, is characterized in that: TiO in polymerize aluminum chloride
2mass content control as 2%-20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310530607.6A CN103979655B (en) | 2013-11-01 | 2013-11-01 | A kind of sewage treatment drug and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310530607.6A CN103979655B (en) | 2013-11-01 | 2013-11-01 | A kind of sewage treatment drug and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN103979655A CN103979655A (en) | 2014-08-13 |
| CN103979655B true CN103979655B (en) | 2015-08-26 |
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|---|---|---|---|
| CN201310530607.6A Expired - Fee Related CN103979655B (en) | 2013-11-01 | 2013-11-01 | A kind of sewage treatment drug and preparation method thereof |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828919B (en) * | 2015-05-14 | 2016-12-07 | 天津鲲鹏化工科技有限公司 | A kind of water treatment agent and preparation method thereof |
| CN104986838B (en) * | 2015-07-02 | 2017-01-11 | 广州弘禹环保科技有限公司 | Preparation method for water treatment agent |
| CN106629884A (en) * | 2016-11-17 | 2017-05-10 | 南京悠谷知识产权服务有限公司 | Water treatment settling agent and preparation method thereof |
| CN108557928A (en) * | 2018-07-22 | 2018-09-21 | 南京市雨花台区绿宝工业设计服务中心 | A kind of preparation method of water treatment agent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197038A (en) * | 1998-04-24 | 1998-10-28 | 中国科学院生态环境研究中心 | High effective polymeric aluminium-silicon chloride flocculant and prepn. tech. thereof |
| JP4164721B2 (en) * | 1999-12-01 | 2008-10-15 | テイカ株式会社 | Flocculant composition for water treatment and use thereof |
| CN101402481A (en) * | 2008-10-16 | 2009-04-08 | 同济大学 | Mesoporous adsorption type aluminum salt composite flocculent synthesis method and uses thereof |
-
2013
- 2013-11-01 CN CN201310530607.6A patent/CN103979655B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197038A (en) * | 1998-04-24 | 1998-10-28 | 中国科学院生态环境研究中心 | High effective polymeric aluminium-silicon chloride flocculant and prepn. tech. thereof |
| JP4164721B2 (en) * | 1999-12-01 | 2008-10-15 | テイカ株式会社 | Flocculant composition for water treatment and use thereof |
| CN101402481A (en) * | 2008-10-16 | 2009-04-08 | 同济大学 | Mesoporous adsorption type aluminum salt composite flocculent synthesis method and uses thereof |
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| CN103979655A (en) | 2014-08-13 |
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Owner name: ZHEJIANG ACADEMY OF AGRICULTURAL SCIENCES Free format text: FORMER OWNER: JI HONGJUN Effective date: 20150701 |
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Inventor after: Yang Shengmao Inventor after: Lv Haohao Inventor after: Liu Yuxue Inventor after: Zhong Zheke Inventor before: Ji Hongjun |
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Free format text: CORRECT: INVENTOR; FROM: JI HONGJUN TO: YANG SHENGMAO LV HAOHAO LIU YUXUE ZHONG ZHEKE |
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Effective date of registration: 20150701 Address after: Hangzhou City, Zhejiang province Jianggan District 310021 Jian Qiao Zhen Shi Qiao Road No. 198 Applicant after: Zhejiang Academy of Agricultural Sciences Address before: A small road in Yuhuatai District of Nanjing City, Jiangsu province 210000 No. 58 Gimpo City family two building two room 505 Applicant before: Ji Hongjun |
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