CN1092141C - Process for preparing active hargil by wet method - Google Patents
Process for preparing active hargil by wet method Download PDFInfo
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- CN1092141C CN1092141C CN99105673A CN99105673A CN1092141C CN 1092141 C CN1092141 C CN 1092141C CN 99105673 A CN99105673 A CN 99105673A CN 99105673 A CN99105673 A CN 99105673A CN 1092141 C CN1092141 C CN 1092141C
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Abstract
The present invention relates to a wet method for producing active white clay, which comprises: after rough separation and pulverization, bentonite reacts with acid at 70 to 100 DEG C for 1.5 to 4.5 hours; products are centrifugally separated and rinsed for a plurality of times and then are neutralized, the pH is controlled, and then, the products are dried and pulverized to obtain products. The wet method for preparing active white clay fully utilizes all washing water and reaction liquid to circularly activate and rinse bentonite, and active white clay and aluminium sulfate can be simultaneously produced. The utilization rate of acid is increased to more than 95%, and the water dosage is only 20% of that of general wet technology. The cost of the production process of the method is reduced by 40%, and the problem of environmental pollution caused by waste water is effectively solved.
Description
The present invention relates to the preparation method of atlapulgite, particularly a kind of preparation method who does not have three wastes wet production high-efficient activated clay.
Atlapulgite is Fuller's earth again, and it is made through artificial activation by natural montmorillonite class clay pit.It is a kind of network of micropores lattice structure that has, and the multi-hole type white powder that specific surface area is very big is a kind of strong sorbent material; Can be used for that oil is concise, the purifying adsorbent of vegetable and animals oils decolouring, deodorizing, transformer oil etc., can also be the raw material of makeup, medicine, coating.Granular atlapulgite can be made the catalyzer of aromatic hydrocarbons reformation, isomerization, disproportionation.Its further processing be can be made into na-pretreated zeolite replaces phosphoric acid salt to be used for detergent industry.
Produce atlapulgite and generally use mineral acid activated bentonite class clay breeze, can be divided into dry method, wet method and semi-wet method according to processing condition.Dry method is with a spot of acid and wilkinite thorough mixing, places certain hour, dries then, pulverizes and form; Its technology is simple, and is free from environmental pollution; Because acid is difficult to be uniformly dispersed with wilkinite, the inorganic salt that reaction is generated can not be removed again, and it is fair relatively poor.Wet method is that water, acid, wilkinite are mixed in reactor by a certain percentage, about 100 ℃, heat 2-6h, reaction product gets atlapulgite through washing, dry, pulverizing, its advantage is that reaction is even and abundant, product performance are stable, decolorizing ability is strong, is the main method of making high-efficient activated clay; Its shortcoming is that acid consumption is big, and water loss is big, cost height, contaminate environment.The patent of this respect has CN1072 869A (1993).In addition, people such as Zhou Shuwen state the method that semi-wet method is produced atlapulgite of having invented, patent No. CN10615 42A, its introduction be with 5% aqueous sulfuric acid in autoclave, in 200-250 ℃ with the 15-20 normal atmosphere under activated bentonite 4 hours; Because used acid concentration is low, cleaning product institute water is fewer, but high temperature, high top pressure operation difficulty has limited applying of it.
The preparation technology who the purpose of this invention is to provide a no three wastes wet production high-efficient activated clay can make full use of the reaction solution of washing water and recovery, reduces production costs, and solves the contaminated wastewater environmental problem.
The preparation method of wet production atlapulgite of the present invention comprise bentonite ore roughly selected, pulverizes after, reacted 1.5-4.5 hour down at 70-100 ℃ with acid, through 3-6 centrifugation and rinsing, then with its neutralization, its PH is controlled at 5-6, and drying, pulverizing promptly get product again.
Wherein, described wilkinite can comprise sodium bentonite, calcium-base bentonite, palygorskite clay, sepiolite clay and attapulgite clay; The granularity of described bentonite is controlled at can pass through the 80-250 mesh sieve.
Described acid can be sulfuric acid, hydrochloric acid or phosphoric acid; The concentration of described acid is at 1.25-4.25mol/L.
Described wilkinite in acid priming reaction in solid-to-liquid ratio be 1: 1.5-2.5.
Described drying course can carry out in air-flow air dryer or converter, air-dryly is less than 8% to moisture and gets final product.
The reaction solution that described reaction back centrifugation goes out can turn back in the reactor with diluted acid as reaction; And the rinsing liquid that goes out through centrifugation after 3-6 time the rinsing can be called a wash water, two wash waters, three wash waters, four wash waters, five wash waters, six wash waters respectively, and wherein, a wash water can be used as reaction and turns back in the reactor with the part of acid; And the later rinse water of two wash waters can be respectively applied for the washing of next process; The controlled water temperature of described washing process is built in 20-80 ℃.
Described N-process is that reaction back material is immersed in the clear water, adds the alkali neutralization, and described alkali can be sodium hydroxid, potassium hydroxide, yellow soda ash, unslaked lime and calcium hydroxide.
Owing to be rich in silico-aluminate in the wilkinite, when adding sulfuric acid, can generate Tai-Ace S 150 with the aluminium reactant salt, therefore, the preparation method of wet production atlapulgite of the present invention can also comprise with reaction solution through concentrate, crystallization produces Tai-Ace S 150 crude product and elaboration, mother liquor is used for the activation of bentonite reaction or is used for sewage disposal.
The preparation method of wet production atlapulgite of the present invention has made full use of whole washing water and reaction solution, circulation is used for activation of bentonite and rinsing, can also produce Tai-Ace S 150 when producing atlapulgite, the utilization ratio of acid is brought up to more than 95%, and the consumption of water only is 20% of a general wet processing, its production process cost of the present invention has reduced by 40%, has solved the contaminated wastewater problem of environment effectively.
The present invention has following advantage compared with prior art:
1, all recycle reaction solution and washing water, removal waste fluid is not free from environmental pollution.
When 2, producing high-efficient activated clay, can obtain byproduct Tai-Ace S 150, one ton of atlapulgite of every production can obtain 0.3 ton in Tai-Ace S 150, has fully utilized wilkinite.
3, the circulation of washing water and reaction solution is used for the washing of activation of bentonite and product, has improved the utilization ratio of water and acid.1.3 tons of one ton of atlapulgite consumption of every production wilkinites; Consume sour 0.25-0.30 ton, the acid consumption descends 40%; Water consumption is 7 tons, reduces to the 15-20% of general wet processing, and production cost is descended.
4, atlapulgite quality homogeneous, the stable performance of producing with preparation method of the present invention, its percent of decolourization and activity degree are all than the product height of general wet production.
Further the present invention is described in detail below in conjunction with embodiment.
Embodiment 1
Adding concentration in reactor is the sulphuric acid soln 1000ml of 1.25mol/L, adds area, Xinghe, Inner Mongol bentonite in powder (crossing 200 mesh sieves) 500g, carries out liquid-solid separation with whizzer at 90-100 ℃ of stirring reaction after 3 hours.Solid is used the 1000ml water rinse at every turn, and centrifuge dripping carries out three times repeatedly; And then soak with the 1000ml clear water, disperse the back to be neutralized to PH=5-6 with 3% aqueous sodium carbonate, centrifuge dripping with the pulverizing of air-flow air dryer, air-dryly be less than 8% to water content, is packed.Its percent of decolourization 95.6%, activity degree 206.The reaction solution that centrifugation goes out is delivered to reactor and is used for the wilkinite activation.Four times washing water divide another name one wash water, two wash waters, three wash waters, four wash waters, and a wash water is used for the wilkinite activation, and all the other are used as the washing of next process product.
Embodiment 2
In reactor, add a wash water (sulfur acid concentration 0.75mol/L) 700ml, reclaim reaction solution (sulfur acid concentration 1.6mol/L) 255ml, vitriol oil 45ml, add area, Xinghe, Inner Mongol wilkinite 450g, carrying out solid, liquid with whizzer at 90-100 ℃ of stirring reaction after 3 hours separates, solid is used two wash waters, three wash waters, four wash waters respectively, and the 1000ml washing dries.Soak, disperse with the 1000ml clear water then, be neutralized to PH=5-6, centrifuge dripping, oven dry, pulverizing with liming.Its percent of decolourization is 99.2%, activity degree 226.The reaction solution that centrifugation goes out is put cold crystallization after evaporating, being concentrated into certain density, obtain Tai-Ace S 150; Its mother liquor claims recovered acid, is used for the wilkinite activation.
Find out relatively that by example 1 and example 2 use the atlapulgite of the reaction solution activated bentonite preparation of washing water and recovery, its quality is better than the clear water complex acid to activation of bentonite.
Embodiment 3
Add a wash water (sulfur acid concentration 0.75mol/L) 930ml in reactor, vitriol oil 70ml added area, Xuanhua, Hebei province wilkinite 500g, 90-100 ℃ of stirring reaction 3 hours.Other operation is with example 2.Gained activated decoloration rate 98.7%, activity degree 221.
Embodiment 4
In reactor, add a wash water (sulfuric acid concentration 0.76mol/L) 550ml, recovered acid (sulfuric acid concentration 1.58mol/L) 400ml, vitriol oil 50ml added area, Yangyuan County, Hebei province wilkinite 500g, 90-100 ℃ of stirring reaction 2.5 hours.Other operation is with example 2.Gained activated decoloration rate 97.6%, activity degree 218.In the reaction solution of activated bentonite, washing water and recovered acid account for 0%-100%.
Claims (9)
1, a kind of preparation method of wet production atlapulgite, it is characterized in that comprising bentonite ore roughly selected, pulverizes after, with acid 70-100 ℃ of reaction 1.5-4.5 hour down, through 3-6 centrifugation and rinsing, with its neutralization, with its PH control 5-6, drying, pulverizing promptly get product more then.
2, preparation method as claimed in claim 1 is characterized in that described wilkinite comprises sodium bentonite, calcium-base bentonite, palygorskite clay, sepiolite clay and attapulgite clay.
3, preparation method as claimed in claim 1, the granularity that it is characterized in that described bentonite is controlled at can pass through the 80-250 mesh sieve.
4 preparation methods as claimed in claim 1 is characterized in that described acid is sulfuric acid, hydrochloric acid or phosphoric acid.
5, preparation method as claimed in claim 1, the concentration that it is characterized in that described acid is at 1.25-4.25mol/L.
6, preparation method as claimed in claim 1 is characterized in that solid-to-liquid ratio is 1 in the priming reaction of described wilkinite in acid: 1.5-2.5.
7, preparation method as claimed in claim 1 is characterized in that described drying course carries out in air-flow air dryer or converter.
8, preparation method as claimed in claim 1 is characterized in that the reaction solution that described reaction back centrifugation goes out turns back in the reactor with diluted acid as reaction; And the rinsing liquid that goes out through centrifugation after 3-6 time the rinsing is called a wash water, two wash waters, three wash waters, four wash waters, five wash waters, six wash waters respectively, and wherein, a wash water is used as reaction and turns back in the reactor with the part of acid; And the later rinse water of two wash waters are respectively applied for the washing of next process; The water temperature of described washing process is controlled at 20-80 ℃.
9, preparation method as claimed in claim 1 is characterized in that described N-process is that reaction back material is immersed in the clear water, adds the alkali neutralization, and described alkali is sodium hydroxid, potassium hydroxide, yellow soda ash, unslaked lime and calcium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99105673A CN1092141C (en) | 1999-04-21 | 1999-04-21 | Process for preparing active hargil by wet method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN99105673A CN1092141C (en) | 1999-04-21 | 1999-04-21 | Process for preparing active hargil by wet method |
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| CN1236732A CN1236732A (en) | 1999-12-01 |
| CN1092141C true CN1092141C (en) | 2002-10-09 |
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| CN99105673A Expired - Fee Related CN1092141C (en) | 1999-04-21 | 1999-04-21 | Process for preparing active hargil by wet method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110013825A (en) * | 2019-04-04 | 2019-07-16 | 深圳清纳科技有限公司 | A kind of activated clay preparation method |
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| WO2008059530A2 (en) * | 2006-11-13 | 2008-05-22 | Chetan Navnithlal Shah | Improved acid treatment process for clay |
| CN102557057B (en) * | 2011-12-28 | 2014-05-14 | 攀枝花学院 | Active argil and preparation method thereof |
| CN106984263A (en) * | 2016-01-20 | 2017-07-28 | 戴祺又 | A kind of modified alta-mud formaldehyde adsorbent and preparation method thereof |
| CN106241823B (en) * | 2016-08-03 | 2017-12-01 | 杨松 | A kind of application method of atlapulgite preparation device special |
| CN106276934B (en) * | 2016-08-03 | 2018-05-08 | 杨松 | One kind prepares atlapulgite rinsing process special purpose device |
| CN106495174B (en) * | 2016-12-02 | 2018-08-07 | 中科院广州能源所盱眙凹土研发中心 | Attapulgite wet method bisgallic acid activation method |
| CN106635250A (en) * | 2016-12-08 | 2017-05-10 | 安徽凯奥新能源股份有限公司 | Method for preparing transformer oil from edible vegetable oil |
| CN109954485A (en) * | 2017-12-26 | 2019-07-02 | 金昌红泉膨润土有限责任公司 | A kind of preparation method of atlapulgite |
| CN109954478A (en) * | 2017-12-26 | 2019-07-02 | 金昌红泉膨润土有限责任公司 | A kind of preparation method of atlapulgite acid lowering agent |
| CN108249452A (en) * | 2018-02-08 | 2018-07-06 | 西南科技大学 | A kind of method that low-temperature bake dry activation prepares atlapulgite |
| CN109110958A (en) * | 2018-08-30 | 2019-01-01 | 黄山市白岳活性白土有限公司 | A kind of hydrochloric acid production atlapulgite waste water treatment process |
| CN116041577A (en) | 2021-10-28 | 2023-05-02 | 中国石油化工股份有限公司 | Olefin polymerization catalyst component, catalyst system, application and olefin polymerization method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054755A (en) * | 1990-03-03 | 1991-09-25 | 国家建材局苏州非金属矿工业设计研究院 | Activation of swelled ground |
| CN1061542A (en) * | 1990-11-21 | 1992-06-03 | 中国矿业大学 | Production method of high-effect and activity clay by semi-hydrometallurgy |
-
1999
- 1999-04-21 CN CN99105673A patent/CN1092141C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054755A (en) * | 1990-03-03 | 1991-09-25 | 国家建材局苏州非金属矿工业设计研究院 | Activation of swelled ground |
| CN1061542A (en) * | 1990-11-21 | 1992-06-03 | 中国矿业大学 | Production method of high-effect and activity clay by semi-hydrometallurgy |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110013825A (en) * | 2019-04-04 | 2019-07-16 | 深圳清纳科技有限公司 | A kind of activated clay preparation method |
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| CN1236732A (en) | 1999-12-01 |
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Assignee: Huangshan Baiyue Activated Clay Co., Ltd. Assignor: Capital Normal Univ. Contract record no.: 2011340000328 Denomination of invention: Process for preparing active hargil by wet method Granted publication date: 20021009 License type: Exclusive License Open date: 19991201 Record date: 20110812 |
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Granted publication date: 20021009 Termination date: 20120421 |