CN1099720A - Preparing method for zinc polysilicate flocculate agent and use - Google Patents
Preparing method for zinc polysilicate flocculate agent and use Download PDFInfo
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- CN1099720A CN1099720A CN 94106231 CN94106231A CN1099720A CN 1099720 A CN1099720 A CN 1099720A CN 94106231 CN94106231 CN 94106231 CN 94106231 A CN94106231 A CN 94106231A CN 1099720 A CN1099720 A CN 1099720A
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- flocculation agent
- zinc
- flocculation
- water
- agent
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Abstract
This invention provides a method for preparing flocculant which uses alkali metal silicate by adding acid, aging and polimerizing, and then adding inorganic zinc salt and assistant. The said flocculant has lower cost than existent aluminium-series and iron-series flocculants, good effect, and no toxic and side effects, and can be used as water purifier for potable water, treating agent for industrialw aste water, and clarifier for sugar refining industry.
Description
The present invention relates to a kind of flocculation agent, particularly with the flocculation agent of polymerization silicate and inorganic zinc salt preparation and in the purposes of water treatment and sugar industry mixing juice clarifying process.
In water and wastewater treatment, inorganic flocculating agent commonly used has aluminium series flocculants (as Tai-Ace S 150, aluminum chloride and polymeric aluminum etc.) and iron series flocculants (as ferrous sulfate, iron trichloride, bodied ferric sulfate etc.), and organic floculant has polyacrylamide and derivative thereof etc.Normal phosphoric acid and the polyacrylamide of using of mixing juice clarification in the sugar industry.
Aluminium series flocculants flocculation ability is strong, be widely used in water and wastewater treatment, but aluminium based flocculating agent production process complexity, the difficult control of condition, the cost height, and in drinking water treatment, be difficult to guarantee that the residual aluminum ion content is below 0.05PPM, many in the world at present countries all in the regulation tap water aluminium composition be not more than 0.05PPM because the tap water aluminium composition is too high HUMAN HEALTH is had potential harm.Iron-based flocculating agent also has good flocculating effect, but Fe
3+Have oxidisability, big to equipment corrosion, the difficult control of water quality causes that easily tap water colourity increases.
It is big that polyacrylamide and derivative thereof have a flco, advantage such as effective, but shortcoming be originate wideless, cost height, and the water security after being difficult to guarantee to handle is harmless.When the mixing juice clarification of sugar industry, use H
3PO
4Easily cause weak points such as equipment corrosion, complicated operation with polyacrylamide.
The objective of the invention is to overcome the weak point of existing inorganic flocculating agent and organic floculant, provide a kind of cost low, purifying water effect is good, widely applicable, production method is simple, harmless polymeric silicicacid zinc class flocculation agent and uses thereof, use this flocculation agent that the water treatment flocculant consumption is reduced, cost reduces, and sucrose letter purity improves, and output increases.
Technical scheme of the invention process is with alkalimetal silicate (aM
2ObSiO
2CH
2O) be mixed into certain pH value ageing reaction with acid earlier as water glass, potassium silicate, water glass, make it to obtain poly-silicic acid, add inorganic zinc salt solution and auxiliary agent then, obtain the liquid zinc polysilicate flocculant at last.The not gelling in 30 days of this flocculation agent, the not gelling in 2-3 month that has guarantees its result of use.
The water glass of the preferred modulus 1.0~4.0 of the above-mentioned alkalimetal silicate of mentioning, used acid are H
2SO
4, HCl, H
2NO
3, HAC etc., used inorganic zinc salt is a content greater than 80% ZnSO
4, ZnCl
2, Zn(NO
3)
2Or ZnO and metallic zinc add the zinc solution that acid obtains, and used auxiliary agent is polyacrylamide and derivative, hexadecyl-octadecyl quaternary ammonium salt etc.
The preparation method of zinc polysilicate of the present invention at first adds 1-10 earlier with alkalimetal silicate doubly to dilute, mix with acid then, the pH value that makes solution is less than 3.0, the ageing reaction is more than 20 hours, add prior dissolved zinc solution again, regulate PH<3.0 with acid, last thin up to finite concentration promptly obtains product, the said products can be at 30 days with interior use, if make storage period long, flocculating effect is more remarkable, can add dissolving good polyacrylamide and 16~octadecyl quaternary ammonium salt earlier in ageing reaction back, adds zinc salt again and transfers PH.
The quality index of the zinc polysilicate flocculant product that aforesaid method makes: proportion is 1.0~2.0, Zn
2+/ SiO
2>0.10, CZn
2+<1.0mol/l, CSiO
2<2.0mol/l, PH<3.0, outward appearance is colourless or white liquid, stationary phase was greater than 30 days.Perhaps contain 0.1%~0.5% polyacrylamide and derivative and 0.1~0.2% 16~octadecyl quaternary ammonium salt in the solution.
Embodiments of the invention:
Embodiment one, to add 28 gram moduluses in the 250ml beaker be 3.1 water glass, adds water 20ml, under agitation mixes with the sulfuric acid of 40 milliliters of 4mol/l then, and re-adjustment PH is 2.5, and ageing of solution was reacted 20 hours, takes by weighing 90% solid ZnCl again
232 grams are dissolved in the 160ml water, mix with the reacted poly-silicate solution of ageing, and use H
2SO
4Or NaOH adjusting PH<3.0, the elimination insolubles promptly obtains about 250 zinc polysilicate flocculants that restrain.This production code member is I type (PSAZ(I) flocculation agent).
Embodiment two, press the poly-silicate solution of method preparation earlier of embodiment one, getting 0.5 gram molecular weight then is dissolved in 50ml hot water greater than 50,000 polyacrylamide acid amide and 0.2 gram hexadecyl quaternary ammonium salt and obtains compounding agent solution, above-mentioned two kinds of solution are all placed more than 20 hours respectively, remerge and stir, other gets 90% solid ZnSO
47H
2O 60 grams are dissolved in the 80ml water, be added to the solution of merging, regulate PH<3.0, the elimination insolubles obtains about 250 zinc polysilicate flocculants that restrain, and this production code member is II type (PSAZ(II) flocculation agent), the gelling phenomenon appears in this product time that may put when growing slightly, be heated to before use about 70 ℃, make its dissolving, use the diluted acid dilution of PH<3.0 to use then.
The application of flocculation agent of the present invention.
1. can be applicable to processing drinking water, replace existing aluminium series water purifier and iron series water purifier, its consumption greatly reduces, and cost reduces, and nontoxic, nothing corrosion safe in utilization.
2. can be applicable to sanitary sewage and industrial sewage and handle, as fibre-bearing and more weaving, papermaking, sugar industry waste water, the waste water of heat-engine plant of impurity, its treatment effect also flocculation agent than other is good.
3. can be applicable to the mixing juice clarifying process of sugar industry, phosphoric acid and polyacrylamide are adopted in mixing juice clarification in existing sugar refinery, the used H of this method clarification
3PO
4And polyacrylamide cost height, and flocculation agent of the present invention can reduce cost, and can also make the simple purity of sugar improve 1%, economic benefit is very remarkable.
4. can use the process that other industry needs flocculation treatment, because this flocculation agent is effective, nontoxic, so the application scenario is very wide.
Flocculation agent of the present invention carries out acute toxicity test in mice through provincial health and epidemic prevention department, its oral dose LD
50>1000mg/kg body weight, the nontoxic level in true border.
Embodiment three, with embodiment one, and the outstanding muddy water sample of the poly-silicic acid flocculation agent I type of example two and the preparation of II type product treatment river silt.(numbering 940055), water sample turbidity 600 degree, colourity 15 degree, PH=7.87 has mud and smells as of rotten fish.Numbering (940057) adds zinc polysilicate flocculant I type product with Zn in the outstanding muddy water sample of 4500ml
2+Ionometer adds 3.75 * 10
-5Mol/l, numbering (940058) adds zinc polysilicate flocculant II type product with Zn in the outstanding muddy water sample of 4500ml
2+Meter adds 2.6 * 10
-5Mol numbers (940056), adds aluminium chlorohydroxide with AL in the outstanding muddy water sample of 4500ml
3+Ionometer adds 7.54 * 10
-5Mol/l.Under 120 rev/mins of rotating speeds, stirred 15 minutes respectively, left standstill 1 hour, draw supernatant liquor 2500ml with sebific duct then and send provincial health and epidemic prevention station to do water quality analysis.Poly-silicic acid flocculation agent and aluminium chlorohydroxide purifying water effect are relatively as the table I.
Table I PSAZ flocculation agent of the present invention and the contrast of aluminium chlorohydroxide purifying water effect
Numbering | The flocculation agent title | Dosage mol/l | Water turbidity (degree) | Colourity (degree) | The PH value | Total hardness CaCO 3mg/l | Total iron mg/l | Total dissolved solid mg/l | Chemical oxygen demand is (in oxygen mg/l |
940055 | 600 | 15 | 7.87 | 128 | 0.83 | 176 | 5.00 | ||
940057 | PSAZ(I) | 3.75×10 -5 | 3.5 | 5 | 8.63 | 146.6 | <0.05 | 211 | 2.84 |
940058 | PSAZ(Ⅱ) | 2.60×10 -5 | 5.0 | 5 | 8.73 | 146.8 | <0.05 | 186 | 3.27 |
940056 | Alkali type aluminium oxide | 7.54×10 -5 | 7.0 | 5 | 8.06 | 138.1 | <0.05 | 348 | 2.72 |
Find out from last table, with the turbid useless water sample turbidity that all is lower than after aluminium chlorohydroxide is handled behind the outstanding muddy water sample of flocculation agent processing of the present invention, various indexs (general physical and chemical index) all reach national drinking water standard, and high slightly PH can not have influence to water quality with small amount of H Cl readjustment PH to 7.0.Explanation thus, flocculation agent of the present invention is a kind of good direct drinking water agent.
Embodiment four, the PSAZ(I) flocculation agent is to the processing of sugar refinery and power plant effluent.The 500ml turbidity be 670 degree to 700 degree, add the PSAZ flocculation agent of 50PPM in the waste water of PH=7.74, use Ca(OH)
2Transfer PH to 8.5, stirred 5 minutes with glass rod then, left standstill 10 minutes, get supernatant liquor then and measure its turbidity less than 10 degree, flocculation efficiency arrives more than 98%.
Embodiment five, get two parts of cane milling mixing juice 500ml, add the 10%PSAZ(I of 1.5ml, 2.0ml respectively) flocculation agent, be warmed up to 55 ℃ and add 15.0ml, the 6%H of 13.0ml more respectively
2SO
3The aqueous solution transfers to PH=8.87 and 8.08 respectively with milk of lime and continues to be warmed up to 100 ℃ of standing sedimentations, measures the volume letter purity of supernatant liquor after 15 minutes, colour, indexs such as turbidity.Control group PSAZ(I) flocculation agent is 1.8ml5%H
3PO
4, temperature, intensity of sulfitation are identical.Experimental result sees Table 2.
Table 2 PSAZ (I) flocculation agent and H
SPO
4Clarification process result contrast
Test number | Flocculation agent | Flocculation agent consumption (ml) | PH value | H 2SO 3Consumption (ml) | Letter purity | Colour ° ST | Turbidity (degree) | Supernatant meter volume (ml) |
A-1 | PSAZ?10% | 1.5 | 8.87 | 15 | 64.95 | 56.15 | 455 | 300 |
B-1 | H 3PO 4?5% | 1.8 | 6.82 | 15 | 62.88 | 47.87 | 827 | 200 |
A-2 | PSAZ?10% | 2.0 | 8.08 | 13 | 65.40 | 82.94 | 455 | 250 |
A-2 | H 3PO 4?5% | 1.8 | 8.03 | 13 | 64.86 | 77.62 | 537 | 190 |
Mixing juice | 5.9 | - | 64.45 | 71.32 | - | - |
See that from the result PSAZ flocculation agent is in simple purity, indexs such as turbidity are better than using H
3PO
4Effect, though a little higher than H of colour
3PO
4Method, but reach the index of producing first sugar, and can reduce colour from improving intensity of sulfitation.So the PSAZ flocculation agent can be used for sugar refinery mixing juice clarifying process, replace H
3PO
4Use, its economic benefit is very remarkable.
Claims (7)
1, a kind of flocculation agent is characterized in that this flocculation agent is alkalimetal silicate (aM
2ObSiO
2CH
2O), as water glass, potassium silicate, water glass after adding sour polymerization and ZnCl
2Or ZnSO
4, Zn (NO
3)
2Or ZnO, metallic zinc add the zinc polysilicate product that inorganic zinc salt reaction that acid makes obtains, and perhaps is added with the zinc polysilicate flocculant of auxiliary agent.
2, flocculation agent according to claim 1 is characterized in that its preparation method is earlier with 1-10 times of water dilution alkalimetal silicate, again with H
2SO
4Or HCl, HNO
3, HAC mixes, the PH that makes solution is less than 3.0, ageing react more than 20 hours, added inorganic zinc salt then, or added auxiliary agent earlier, added inorganic zinc salt again, or added auxiliary agent earlier, added inorganic zinc salt again and reacted and obtain.
3,, it is characterized in that being polyacrylamide and derivative and 16~octadecyl quaternary ammonium salt according to claim 1 and 3 described flocculation agents.
4,, it is characterized in that the content of this flocculation agent is according to claim 1 and 3 described flocculation agents:
Zn
2+/ SiO
2>0.1, CZn
2+<1.0 mol/l, CSiO
2<2.0 mol/l, its auxiliary agent content: polyacrylamide is 0.1~0.3%, 16-octadecyl quaternary ammonium salt is 0.1~0.2%.
5, flocculation agent according to claim 1 is characterized in that the purposes of zinc polysilicate as the tap water flocculation agent.
6, flocculation agent according to claim 1 is characterized in that the purposes of zinc polysilicate as life or Industrial Wastewater Treatment flocculation agent.
7, flocculation agent according to claim 1 is characterized in that zinc polysilicate is as replacing sugar industry finings H
3PO
4Work way with polyacrylamide and derivative thereof.
Priority Applications (1)
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---|---|---|---|
CN94106231A CN1036774C (en) | 1994-06-03 | 1994-06-03 | Preparing method for zinc polysilicate flocculate agent and use |
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CN94106231A CN1036774C (en) | 1994-06-03 | 1994-06-03 | Preparing method for zinc polysilicate flocculate agent and use |
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CN1099720A true CN1099720A (en) | 1995-03-08 |
CN1036774C CN1036774C (en) | 1997-12-24 |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1091468C (en) * | 2000-03-30 | 2002-09-25 | 华南理工大学 | Magnetic defecation method of natural sugar liquor |
CN103933960A (en) * | 2014-03-18 | 2014-07-23 | 中原工学院 | Preparation method and application of polyzinc silicate doped hydroxy zinc oxide catalyst |
CN104379514A (en) * | 2012-06-26 | 2015-02-25 | 荷兰联合利华有限公司 | Water clarification composition and process |
CN107324471A (en) * | 2017-08-30 | 2017-11-07 | 云南磷化集团有限公司 | A kind of phosphorus ore special efficient flocculant |
CN108017133A (en) * | 2017-12-23 | 2018-05-11 | 安徽睿知信信息科技有限公司 | A kind of municipal sewage treatment flocculant and its manufacture method |
CN110791593A (en) * | 2018-08-03 | 2020-02-14 | 广西科技大学 | Method for decoloring sugar juice by using water-soluble magnesium salt-lime |
CN110904280A (en) * | 2018-09-18 | 2020-03-24 | 广西科技大学 | Method for decoloring sugar juice by using water-soluble zinc salt-lime |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SU805952A3 (en) * | 1977-09-06 | 1981-02-15 | Циба-Гейги Аг (Фирма) | Method of preparing metal silicate for polymer |
US4676929A (en) * | 1985-06-10 | 1987-06-30 | Corning Glass Works | Gels, gel products and methods |
JPS63130189A (en) * | 1986-11-21 | 1988-06-02 | Suido Kiko Kk | Water treatment method and flocculating agent used therefor |
FR2673930B1 (en) * | 1991-03-14 | 1993-08-27 | Inst Francais Du Petrole | NOVEL 2: 1 DIOCTRAEDRIC PHYLLOSILICATES AND THEIR PREPARATION PROCESS. |
FR2682371B1 (en) * | 1991-10-09 | 1993-11-26 | Institut Francais Petrole | 2: 1 TRIOCTAEDRIC PHYLLOSILICATES AND THEIR PREPARATION PROCESS. |
CN1091393A (en) * | 1994-01-13 | 1994-08-31 | 沈阳化工学院 | Method with Water Quenching Slag or flying dust production silicic acid based flocculating agent |
-
1994
- 1994-06-03 CN CN94106231A patent/CN1036774C/en not_active Expired - Fee Related
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1091468C (en) * | 2000-03-30 | 2002-09-25 | 华南理工大学 | Magnetic defecation method of natural sugar liquor |
CN104379514A (en) * | 2012-06-26 | 2015-02-25 | 荷兰联合利华有限公司 | Water clarification composition and process |
CN103933960A (en) * | 2014-03-18 | 2014-07-23 | 中原工学院 | Preparation method and application of polyzinc silicate doped hydroxy zinc oxide catalyst |
CN107324471A (en) * | 2017-08-30 | 2017-11-07 | 云南磷化集团有限公司 | A kind of phosphorus ore special efficient flocculant |
CN108017133A (en) * | 2017-12-23 | 2018-05-11 | 安徽睿知信信息科技有限公司 | A kind of municipal sewage treatment flocculant and its manufacture method |
CN110791593A (en) * | 2018-08-03 | 2020-02-14 | 广西科技大学 | Method for decoloring sugar juice by using water-soluble magnesium salt-lime |
CN110904280A (en) * | 2018-09-18 | 2020-03-24 | 广西科技大学 | Method for decoloring sugar juice by using water-soluble zinc salt-lime |
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