CN100586852C - Method for producing organic clay - Google Patents
Method for producing organic clay Download PDFInfo
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- CN100586852C CN100586852C CN200610049660A CN200610049660A CN100586852C CN 100586852 C CN100586852 C CN 100586852C CN 200610049660 A CN200610049660 A CN 200610049660A CN 200610049660 A CN200610049660 A CN 200610049660A CN 100586852 C CN100586852 C CN 100586852C
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- quaternary ammonium
- ammonium salt
- clay
- organic clay
- methyl chloride
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Abstract
The present invention discloses organic clay producing process, which includes the steps of: pulping clay mineral, deposition and centrifuging purification to obtain clay suspension; preparing quaternary ammonium salt aqua of 10-30 wt% concentration with tertiary amine as material, water as solvent and introduced chloromethane; adding quaternary ammonium salt aqua into clay suspension for modification; and dewatering the modified solution, drying and crushing to obtain organic clay product. Thus produced organic clay product has high quality and the production process has low waste water CODCrindex, and is one clean low-cost production process.
Description
Technical field
The present invention relates to a kind of production method of material, especially relate to a kind of production method of organic clay of modification.
Background technology
The technology of producing at present both at home and abroad organic clay generally comprises following processing step: raw ore clay wet method is disperseed, remodeling, purify, and the suspension after the purification is with quaternary ammonium salt-modified, the dehydration that contains organic solvent, dry and divide grade packaged.
Adopt the organic clay stay in grade of this explained hereafter, but properties-correcting agent adopts the quaternary ammonium salt solution more than 70% usually, after cation quaternary ammonium salt is adsorbed by clay, also have 20～25% organic solvents (as ethanol, methyl alcohol, Virahol etc.) not to be adsorbed.These solvents enter trade effluent in dehydration procedure, make COD
CrReach 2500～4000mg/L, bring ambient water to pollute.
Application for a patent for invention 00101420.X discloses a kind of production method of organic bentonite, and its steps in sequence is ore dressing, pulverizing is selected, extrusion process is organically-modified, drying and crushing and finished product packing.Adopting 12-octadecyl quaternary amine in the extrusion modification is that insulating covering agent is extruded on screw extrusion press.
Application for a patent for invention 03116258.4 discloses the synthetic bentonite method of a kind of microwave, 20～the 200%CEC of cation exchange capacity that tensio-active agent is pressed the wilkinite original soil is soluble in water, its quality solid-to-liquid ratio scope was at 1: 5～1: 500, the wilkinite original soil that add drying, sieves, put into the microwave reactor of 100～5000W microwave power, irradiation 10s-30min, overanxious, flush away free tensio-active agent, microwave drying, in 60～120 ℃ of oven dry down, drying time is 30min～24hr, grind, sieve, obtain organobentonite.
In the above-mentioned technology, because a large amount of uses of alcoholic solvent, need hold concurrently oxygen or anaerobism, oxygen consumption Wastewater Treated by Activated Sludge Process of trade effluent simultaneously, these two aspects improve production cost greatly.
Patent of invention ZL02103804.X discloses a kind of dry-process method for producing bentonite, the main organobentonite that the natural calcium base bentonite is become high value by the artificial modification that is suitable for.Be that the natural calcium base bentonite is added soda ash in mixing facilities, permutoid reaction generates sodium bentonite, adds activator then, mixing, reaction; Add organic insulating covering agent again, fully heating, mixing, reaction.Be extruded into bar with screw extrusion press at last, extrudate drying, abrasive dust become the organobentonite powder.
Though this technology does not produce or only produce a small amount of trade effluent, quaternary ammonium salt still contains a large amount of organic solvents, and volatilizees with water vapour in drying process and enter air, air is polluted, and be difficult to administer, and or not the method for cleaner production; In addition, because the dry process extent of purification is not high, the organobentonite quality product is not high, and the use range of product is restricted.
Summary of the invention
The invention provides the production method of a kind of cleaning, organic clay that cost is low.
A kind of production method of organic clay may further comprise the steps:
(1) to the raw ore clay pull an oar, sedimentation and centrifugal purification, make slurry; Cationic exchange total amount is in the slurry of purification back: (a) wilkinite, the single mineral of hectorite are 90～130mmol/100g; (b) sepiolite, kaolin, the single mineral of Attapulgite are more than the 20mmol/100g; (c) multiple clay mixing suspension according to the ratio difference, need reach 50～130mmol/100g;
(2) slurry that makes is heated to 75～95 ℃, the quaternary ammonium salt add-on is 0.8～1.2 times of slurry cationic exchange total amount, and adding content is 10～30% quaternary ammonium salt aqueous solution, carries out modified-reaction 0.5～2 hour under 60～95 ℃;
(3) to the solution after the modification dewater, dry, pulverize, divide the grade packaged finished product that makes.
Described raw ore clay be sodium base or calcium-base bentonite, sepiolite, hectorite, Attapulgite, kaolinic one or more.
Described content is the preparation method of 10～30% quaternary ammonium salt aqueous solution, may further comprise the steps: the water of in conversion unit, packing into, be steam heated to 65～75 ℃, and be 1: 2.5～4.0 in the ratio of tertiary amine and water, drop into C
12-C
18Tertiary amine, insulated and stirred fed methyl chloride 2～6 hours down at 60～95 ℃, and reaction is to terminal.
Described C
12-C
18Tertiary amine is one or more of 12,14,16,18 tertiary amines.
Described conversion unit is the airtight reactor that recycle pump and spray equipment or machinery stir device of being furnished with.
The organic clay good product quality that technology produced according to the invention makes, because not with an organic solvent, COD in the waste water
CrIndex reaches discharging standards, and the processing of sewage need not adopted double oxygen (or anaerobism), activated sludge method processing technique, greatly reduces production cost.
Embodiment
A kind of production method of organic clay may further comprise the steps:
(1) preparation slurry
With the making beating of raw ore clay, the control solid content is 10～20%, thin up to 2～10%, and natural subsidence is more than 4 hours, and upper strata suspension adopts the centrifugal purification of whizzer, and the suspension solid content after the purification is controlled at 1.0～3.0g/100ml.The raw ore clay can be sodium base or calcium-base bentonite, sepiolite, hectorite, Attapulgite, kaolinic one or more, cationic exchange total amount is in the back slurry of purifying: (1) wilkinite, the single mineral of hectorite are 90～130mmol/100g; (2) sepiolite, kaolin, the single mineral of Attapulgite are more than the 20mmol/100g; (3) multiple clay mixing suspension according to the ratio difference, need reach between 50～130mmol/100g.
(2) preparation 10～30% quaternary ammonium salt aqueous solutions
In the 3000L reactor, add 1500～2200kg tap water in advance, be steam heated to 65～75 ℃ with chuck or coil pipe, drop into 12 again, 14,16,18 tertiary amines or mixing tertiary amine 540～570kg, start and stir or the ON cycle pump, continue heat tracing, open the methyl chloride pressure loading valve, slowly in reactor, fed methyl chloride 2～6 hours, control ventilation speed, temperature of reaction progressively rises in the reaction process, when temperature rises to 95 ℃, steam off, and prepare to pour cold water with controlled temperature to chuck, when the value of the reactant amine in the reactor＜0.1mg/g, get final product.In the reaction process, the air pressure in the reactor is controlled at below the 0.3Mpa.s, and keeps aeration time 2～4 hours, and it is 90～110 kilograms that methyl chloride feeds quantity.
(3) preparation organic clay
The slurry of step (1) preparation is heated to 75～95 ℃, and to transfer pH value be 3～5, press slurry total cation exchange capacity 0.8～1.2 times, 10～30% the quaternary ammonium salt aqueous solution that makes in the adding step (2), modified-reaction 0.5～2 hour; To the solution behind the modified-reaction dewater, dry, pulverize, divide the grade packaged organic clay of making.
Embodiment 1:
(1) getting soil ratio is 10: 1 wilkinite raw ore, pulls an oar after 2 hours, add the remodeling auxiliary agent and continued again to pull an oar 3 hours, and diluted settlement 4 hours, upper strata suspension is purified with whizzer, and differential 15, rotating speed are 2500r/min, flow 20m
3/ h.Slurry solid content after the purification is 2.4g/100ml, solids content 120kg, cation exchange capacity 92mmol/100g.
(2) in 3000L have chuck and be furnished with recycle pump and the reactor of spray equipment in, add tap water 2200kg, and be heated to 65 ℃ with steam jacket, drop into 18/16 tertiary amine mixture 560kg, wherein C
18Account for 68.2%, C
16Account for 27.1%.ON cycle pump spray is opened methyl chloride steel cylinder reducing valve, slowly feeds methyl chloride, and along with reaction is carried out, temperature rises to 90 ℃ gradually, and the air pressure in the reactor is controlled at below the 0.3Mpa.s, can be by closing methyl chloride or reducing temperature and control.Fed methyl chloride 4 hours, sampling analysis amine value, the amine value is 0.07mg/g, is reacted to terminal point.The air flow of methyl chloride is 95kg, and after tested, the content of quaternary ammonium salt is 22.4%, and this batch quaternary ammonium salt aqueous solution is standby.
(3) slurry that (1) is prepared is heated to 85 ℃, drops into 22.4% quaternary ammonium salt aqueous solution 171kg, and it is 1: 1 with total ion exchange capacity that quaternary ammonium salt adds mole number, react 1 hour, dehydration, dry, pulverize, branch is grade packaged.
After tested, trade effluent COD
CrBe 91mg/L; Product is pressed HG/T2248 standard testing I class viscosity 6.3Pa.s.
Embodiment 2:
(1) getting wilkinite raw ore and sepiolite is to mix at 2: 1 by weight, drop into making beating, water: soil is 15: 1, pulls an oar 1 hour, continues making beating 3 hours behind the input remodeling auxiliary agent, being diluted with water to solid content is 5%, stir sedimentation after 6 hours, carry out centrifugal purification, purification rear suspension liquid test solid content 1.8g/100ml by step (1) among the embodiment 1, admittedly contain total amount 90kg, cationic exchange total amount 77mmol/100g.
(2) slurry for preparing in (1) is heated to 85 ℃,, adds the quaternary ammonium salt aqueous solution 108kg of step (2) among the embodiment 1, react 0.5 hour by 0.8 times of cationic exchange total amount, again through dehydration, dry, pulverize, branch is grade packaged.
Trade effluent COD in this example
CrBe 72mg/L; Product is 3.5Pa.s by HG/T2248 standard testing I class viscosity.
Embodiment 3:
(1) gets wilkinite raw ore and Attapulgite, be input making beating in 3: 1 by weight, water: soil is 15: 1, pulls an oar 2 hours, continues making beating 2 hours behind the input remodeling auxiliary agent, being diluted with water to solid content is 4%, stir sedimentation after 6 hours, carry out centrifugal purification, purification rear suspension liquid test solid content 1.2g/100ml by step (1) among the embodiment 1, admittedly contain total amount 100kg, cationic exchange total amount 85mmol/100g.
(2) in 3000L have chuck and be furnished with recycle pump and the reactor of spray equipment in, add tap water 1500kg, and be heated to 65 ℃ with steam jacket, drop into C
18, C
16, C
14, C
12Tertiary amine mixture 540kg, wherein C
18Account for 70%, C
16Account for 23%, C
14Account for 4.5%, C
12Account for 1.5%.ON cycle pump spray is opened methyl chloride steel cylinder reducing valve, slowly feeds methyl chloride, and along with reaction is carried out, temperature rises to 90 ℃ gradually, and the air pressure in the reactor is controlled at below the 0.3Mpa.s, can be by closing methyl chloride or reducing temperature and control.Fed methyl chloride 4 hours, sampling analysis amine value, the amine value is 0.07mg/g, is reacted to terminal point.The air flow of methyl chloride is 90kg, and after tested, the content of quaternary ammonium salt is 28%, and this batch quaternary ammonium salt aqueous solution is standby.
(2) slurry for preparing in (1) is heated to 75 ℃,, adds the quaternary ammonium salt aqueous solution 104kg of above-mentioned steps (2), react 1 hour by 1 times of cationic exchange total amount, again through dehydration, dry, pulverize, branch is grade packaged.
Trade effluent COD in this example
CrBe 81mg/L; Product is 3.0Pa.s by HG/T2248 standard testing I class viscosity.
Embodiment 4:
(1) getting wilkinite raw ore and kaolin is 2: 1 by weight, drop into making beating, water: soil is 1: 10, pulls an oar 2 hours, continues making beating 3 hours behind the input remodeling auxiliary agent, being diluted with water to solid content is 45g/100ml, stir sedimentation after 6 hours, carry out centrifugal purification, purification rear suspension liquid test solid content 2.8g/100ml by step (1) among the embodiment 1, admittedly contain total amount 40kg, cationic exchange total amount 56mmol/100g.
(2) in 3000L have chuck and be furnished with recycle pump and the reactor of spray equipment in, add tap water 2200kg, and be heated to 65 ℃ with steam jacket, drop into C
18, C
16Tertiary amine mixture 540kg, wherein C
18Account for 71%, C
16Account for 28%.ON cycle pump spray is opened methyl chloride steel cylinder reducing valve, slowly feeds methyl chloride, and along with reaction is carried out, temperature rises to 90 ℃ gradually, and the air pressure in the reactor is controlled at below the 0.3Mpa.s, can be by closing methyl chloride or reducing temperature and control.Fed methyl chloride 4 hours, sampling analysis amine value, the amine value is 0.10mg/g, is reacted to terminal point.The air flow of methyl chloride is 93.8kg, and after tested, the content of quaternary ammonium salt is 17.8%, and this batch quaternary ammonium salt aqueous solution is standby.
(3) slurry for preparing in (1) is heated to 90 ℃,, adds the quaternary ammonium salt aqueous solution 152.6kg of above-mentioned steps (2), react 2 hours by 0.8 times of cationic exchange total amount, again through dehydration, dry, pulverize, branch is grade packaged.
Trade effluent COD in this example
CrBe 61mg/L; Product is 5.2Pa.s by HG/T2248 standard testing I class viscosity.
Embodiment 5:
(1) getting wilkinite and hectorite is 1: 1 by weight, drop into making beating, water: soil is 10: 1, pulls an oar 2 hours, continues making beating 3 hours behind the input remodeling auxiliary agent, being diluted with water to solid content is 4.2g/100ml, stir sedimentation after 6 hours, carry out centrifugal purification, purification rear suspension liquid test solid content 2.2g/100ml by step (1) among the embodiment 1, admittedly contain total amount 110kg, cationic exchange total amount 125mmol/100g.
(2) in 3000L have chuck and be furnished with recycle pump and the reactor of spray equipment in, add tap water 2200kg, and be heated to 65 ℃ with steam jacket, drop into C
18, C
16, C
14Tertiary amine mixture 570kg, wherein C
18Account for 68.2%, C
16Account for 24.3%, C
14Account for 5%.ON cycle pump spray is opened methyl chloride steel cylinder reducing valve, slowly feeds methyl chloride, and along with reaction is carried out, temperature rises to 90 ℃ gradually, and the air pressure in the reactor is controlled at below the 0.3Mpa.s, can be by closing methyl chloride or reducing temperature and control.Fed methyl chloride 4 hours, sampling analysis amine value, the amine value is 0.09mg/g, is reacted to terminal point.The air flow of methyl chloride is 110kg, and after tested, the content of quaternary ammonium salt is 24.2%, and this batch quaternary ammonium salt aqueous solution is standby.
(3) slurry for preparing in (1) is heated to 95 ℃,, adds the quaternary ammonium salt aqueous solution 191kg of step (2), react 2 hours by 1.2 times of cationic exchange total amount, again through dehydration, dry, pulverize, branch is grade packaged.
Trade effluent COD in this example
CrBe 97mg/L; Product is 4.5Pa.s by HG/T2248 standard testing I class viscosity.
Embodiment 6:
(1) get wilkinite: hectorite: sepiolite: the Attapulgite ratio is 2: 2: 1: 1, drop into making beating, water: soil is 10: 1, pulls an oar 2 hours, continues making beating 3 hours behind the input remodeling auxiliary agent, being diluted with water to solid content is 4.0g/100ml, stir sedimentation after 6 hours, carry out centrifugal purification, purification rear suspension liquid test solid content 1.2g/100ml by step (1) among the embodiment 1, admittedly contain total amount 70kg, cationic exchange total amount 80mmol/100g.
(2) in 3000L have chuck and be furnished with recycle pump and the reactor of spray equipment in, add tap water 2200kg, and be heated to 65 ℃ with steam jacket, drop into C
18, C
16Tertiary amine mixture 540kg, wherein C
18Account for 30%, C
16Account for 70%, C
14Account for 2.5%.ON cycle pump spray is opened methyl chloride steel cylinder reducing valve, slowly feeds methyl chloride, and along with reaction is carried out, temperature rises to 90 ℃ gradually, and the air pressure in the reactor is controlled at below the 0.3Mpa.s, can be by closing methyl chloride or reducing temperature and control.Fed methyl chloride 4 hours, sampling analysis amine value, the amine value is 0.08mg/g, is reacted to terminal point.The air flow of methyl chloride is 95kg, and after tested, the content of quaternary ammonium salt is 25.1%, and this batch quaternary ammonium salt aqueous solution is standby.
(3) slurry for preparing in (1) is heated to 90 ℃,, adds the quaternary ammonium salt aqueous solution 78kg of step (2) among the embodiment 1, react 0.5 hour by 1 times of cationic exchange total amount, again through dehydration, dry, pulverize, branch is grade packaged.
Trade effluent COD in this example
CrBe 62mg/L; Product is 3.1Pa.s by HG/T2248 standard testing I class viscosity.
Embodiment 7:
(1) gets sepiolite, drop into making beating, water: soil is 10: 1, pulls an oar 2 hours, continues making beating 3 hours behind the input remodeling auxiliary agent, being diluted with water to solid content is 3.2g/100ml, stir sedimentation after 6 hours, carry out centrifugal purification, purification rear suspension liquid test solid content 1.2/100ml by step (1) among the embodiment 1, admittedly contain total amount 60kg, cationic exchange total amount 36mmol/100g.
(2) in 3000L have chuck and be furnished with recycle pump and the reactor of spray equipment in, add tap water 2200kg, and be heated to 65 ℃ with steam jacket, drop into C
18Tertiary amine mixture 560kg, wherein C
18Account for 95.80%, C
16Account for 2.3%.ON cycle pump spray is opened methyl chloride steel cylinder reducing valve, slowly feeds methyl chloride, and along with reaction is carried out, temperature rises to 90 ℃ gradually, and the air pressure in the reactor is controlled at below the 0.3Mpa.s, can be by closing methyl chloride or reducing temperature and control.Fed methyl chloride 4 hours, sampling analysis amine value, the amine value is 0.07mg/g, is reacted to terminal point.The air flow of methyl chloride is 95kg, and after tested, the content of quaternary ammonium salt is 22.5%, and this batch quaternary ammonium salt aqueous solution is standby.
(3) slurry for preparing in (1) is heated to 90 ℃,, adds the quaternary ammonium salt aqueous solution 33.4kg of step (2), react 2 hours by 1 times of cationic exchange total amount, again through dehydration, dry, pulverize, branch is grade packaged.
Trade effluent COD in this example
CrBe 72mg/L; Product is 2.1Pa.s by HG/T2248 standard testing I class viscosity.
Claims (3)
1, a kind of production method of organic clay may further comprise the steps:
(1) in sodium base or calcium-base bentonite, sepiolite, hectorite, Attapulgite, the kaolin surpass a kind of raw ore clay be mixed in proportion pull an oar, sedimentation and centrifugal purification, make slurry, cationic exchange total amount is 50～130mmol/100g in the slurry;
(2) suspension that makes is heated to 75～95 ℃, the quaternary ammonium salt add-on is 0.8～1.2 times of slurry cationic exchange total amount, and adding content is 10～30% quaternary ammonium salt aqueous solution, carries out modified-reaction 0.5～2 hour under 60～95 ℃;
The preparation method of described quaternary ammonium salt aqueous solution may further comprise the steps: the water of in conversion unit, packing into, be steam heated to 65～75 ℃, and be 1: 2.5～4.0 by the weight ratio of tertiary amine and water, drop into C
12-C
18Tertiary amine, insulated and stirred fed methyl chloride 2～6 hours down at 60～95 ℃, and reaction is to terminal;
(3) to the solution after the modification dewater, dry, pulverize, divide the grade packaged finished product that makes.
2, the production method of organic clay as claimed in claim 1 is characterized in that: described C
12-C
18Tertiary amine is one or more of 12,14,16,18 tertiary amines.
3, the production method of organic clay as claimed in claim 1 is characterized in that: described conversion unit is the airtight reactor that recycle pump and spray equipment or machinery stir device of being furnished with.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610049660A CN100586852C (en) | 2006-03-01 | 2006-03-01 | Method for producing organic clay |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610049660A CN100586852C (en) | 2006-03-01 | 2006-03-01 | Method for producing organic clay |
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|---|---|
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| CN100586852C true CN100586852C (en) | 2010-02-03 |
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ID=36922675
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|---|---|---|---|
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055801A (en) * | 2012-12-18 | 2013-04-24 | 华南理工大学 | Alkylamine modified inorganic clay mineral adsorbing material, and preparation method as well as application of same |
| CN104561147B (en) * | 2013-10-22 | 2017-08-22 | 中国石油化工股份有限公司 | A kind of sterilizing methods of liquid alkane |
| CN104561138B (en) * | 2013-10-22 | 2017-08-22 | 中国石油化工股份有限公司 | A kind of preprocess method of liquid alkane for biofermentation |
| CN105905915B (en) * | 2016-04-14 | 2018-02-02 | 浙江红宇新材料股份有限公司 | A kind of preparation method of Bentonite modifier |
| WO2018204620A1 (en) | 2017-05-05 | 2018-11-08 | Active Minerals International, Llc | Composition to completely or partially replace ball clay in ceramics, method of making, and use thereof |
| CN107082434B (en) * | 2017-05-08 | 2019-12-13 | 中国地质大学（北京） | One-step process for purifying and organically modifying sepiolite |
| CN112301791B (en) * | 2020-08-21 | 2022-07-12 | 浙江杭化新材料科技有限公司 | Preparation method of vat sticking agent for household paper |
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