CN1415721A - Technical method for producing P type zeolite for washing use by activating bentonite with alkaline process being utilized - Google Patents

Technical method for producing P type zeolite for washing use by activating bentonite with alkaline process being utilized Download PDF

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CN1415721A
CN1415721A CN 02156482 CN02156482A CN1415721A CN 1415721 A CN1415721 A CN 1415721A CN 02156482 CN02156482 CN 02156482 CN 02156482 A CN02156482 A CN 02156482A CN 1415721 A CN1415721 A CN 1415721A
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bentonite
type washing
liquid
crystallization
washing zeolite
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CN1162527C (en
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曹吉林
谭朝阳
李春旭
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Hebei University of Technology
Hebei Polytechnic University
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Hebei University of Technology
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Abstract

A process for preparing P-type zeolite for washing products from bentonite activated by alkali method includes such steps as purifying, activating by alkali, dissolving in water, regulating the mole ratio of SiO2, Al2O3 and Na2O, reaction, ageing, and crystallizing. Its advantages are high speed for extracting Si and Al, short activating time, and low cost.

Description

The alkaline process activated bentonite is produced the processing method of P type washing zeolite
Technical field of the present invention
The invention belongs to a kind of preparation method of P type washing zeolite, particularly a kind of alkaline process activated bentonite is produced the processing method of P type washing zeolite.
Background technology of the present invention
Wilkinite is a kind of hydrous alumino silicates earthy mineral, has rich in natural resources in China, existing 11.25 hundred million tons of proven reserve, and produced quantity is 2,000,000 tons at present.Bentonitic main chemical compositions is SiO 2And Al 2O 3, contain the oxide compound of small amount of calcium, magnesium, iron etc. in addition.Because it has special laminate structure and physicochemical property, so be widely used in each departments such as metallurgy, precision casting, oil production, refining of petroleum, daily-use chemical industry, chemical building material, paint.Yet calcium-base bentonite, sodium bentonite and three kinds of primary products of atlapulgite are made by China's wilkinite overwhelming majority of exploitation at present, and this traditional industries are low in economic efficiency, fully do not excavate bentonitic value.So current common recognition that the transformation and upgrade of wilkinite processing industry has been become people.
At present relevant wilkinite deep processing research, generally adopt the method for acid activation to destroy its laminate structure, make the silicon in the wilkinite be transformed into active silica, aluminium is transformed into aluminum soluble salt, and then the deep processed product by obtaining wanting with other substance reactions or CONTROL PROCESS condition.Leaching rate and leaching yield that this deep processing technology exists sial are low, soak time is long, the bad processing of spent acid solution, technical process is than shortcomings such as complexity, therefore, flexibly, not cause the processing method of secondary pollution be urgent and necessary to a kind of, product category simple to bentonite resource utilization ratio height, production technique of research.
Technology contents of the present invention
Technical problem to be solved by this invention is to overcome weak point of the prior art, provides a kind of alkaline process activated bentonite to produce the processing method of P type washing zeolite.This method can be improved the wilkinite deep processing technology, and resource utilization is improved, and production cost reduces, and product category is flexible, realizes producing pollution-free.
Technical solution of the present invention is as follows:
Alkaline process activated bentonite of the present invention is produced the processing method of P type washing zeolite, and its processing step is as follows:
1, purify: bentonite is washed, removal of impurities, oven dry, standby after the pulverization process;
2, alkali fusion activation: will after wilkinite after the pulverization process and caustic soda (sodium hydroxide) pressed powder mix, carry out the processing of alkali fusion activating process;
3, water dissolution-mode transfer-reaction is aging: the activation raw material after the alkali fusion activating process is handled is adjusted Al through water dissolution 2O 3, SiO 2, Na 2O, H 2The mol ratio of O is reacted burin-in process after being suitable proportion;
4, crystallization: will carry out the crystallization processing through the feed liquid of reacting after wearing out;
5, solid-liquid separation: the feed liquid after crystallization is carried out solid-liquid separation, and liquid phase is delivered to water dissolution-mode transfer-reaction aging technique section, is used to adjust Al 2O 3, SiO 2, Na 2O, H 2The mol ratio of O, solid phase are P type washing zeolite;
6, solid phase is handled: will be after solid-liquid separation the gained solid phase, wash, wash water is delivered to water dissolution-mode transfer-reaction aging technique section, is used to adjust Al 2O 3, SiO 2, Na 2O, H 2The mol ratio of O, the filter cake drying, pulverization process promptly obtains P type washing zeolite product.
The grinding particle size of bentonite described in the above-mentioned processing step before washing is 120 orders-200 orders.
Purifying technique described in the above-mentioned processing step is handled, and is the dilute slurry that grinding particle size 120 orders-200 purpose bentonite is mixed with, and through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 120 orders-200 order and promptly gets the back bentonite of purifying.
Alkali fusion activating process described in the above-mentioned processing step, be will be after purifying bentonite and caustic soda (sodium hydroxide) press mass ratio 1: 1-1: 1.6 batchings, mix the back and in 300 ℃-600 ℃ retort furnace, reacted 1-6 hour, promptly obtain Powdered activation back grog.
Water dissolution-mode transfer described in the above-mentioned processing step-reaction aging technique is with the grog after alkali fusion activating process activation and aluminium hydroxide, water, presses Al 2O 3: SiO 2: Na 2O: H 2O :=1: (1.8-2.3): (2.9-3.2): (170-220) feed intake after, under 40 ℃-100 ℃ aging temperature aging 2-8 hour, promptly get the original liquid for preparing P type washing zeolite.
Crystallization process described in the above-mentioned processing step is the crystal seed that original liquid after handling through the reaction aging technique drops into 0.5%-7%, under 60 ℃-120 ℃ temperature crystallization 5-24 hour, promptly gets the product feed liquid.
Solid-liquid separation described in the above-mentioned processing step, be solid phase with gained through deionized water wash to PH=7-8, promptly obtain filter cake, the filter cake drying promptly gets P type washing zeolite product after the pulverizing.
The present invention compared with prior art has following advantage:
1, improved the utilization ratio of bentonite resource, the alkali fusion activating process makes that the utilization ratio of silicon-dioxide and aluminium sesquioxide reaches more than 90% in the wilkinite among the present invention.
2. adopt the alkali fusion activated bentonite, avoid in the present acid system activating process soak time long, the sial leaching yield is low, and shortcomings such as the bad processing of spent acid solution make the technology of wilkinite deep processing system zeolite more reasonable.
3. the present invention adopts the alkali fusion activating process, sial utilization ratio height, and production elasticity is big, can be according to Al in the dissimilar zeolite molecular sieve synthesis systems 2O 3, SiO 2, Na 2O, H 2The proportioning of O is adjusted, selection production adaptation market, the product that competitive power is strong.
4. the P type washing zeolite of explained hereafter of the present invention has overcome the shortcoming of 4A zeolite to the magnesium ion exchange capacity difference, not only calcium magnesium there is good ion exchange, but also has the stability of some more expensive recipe ingredient in very high nonionogenic tenside loading capacity and the raising washing composition.Thereby P type zeolite is considered to the substitute products of 4A zeolite as the tool potentiality of washing auxiliary detergent.
The drawing explanation of accompanying drawing
Fig. 1 is a technological process of production synoptic diagram of the present invention;
Fig. 2 is a product P type molecular sieve X diffractogram of the present invention.
Bentonite origin breeze among Fig. 1 is meant with the montmorillonite to be that the clay mineral (wherein silicon-dioxide accounts for 50%-75%, and aluminium sesquioxide accounts for 8%-17%) of main component makes through mechanical disintegration.The grinding particle size requirement of bentonite origin breeze before washing is 120 orders-200 orders among Fig. 1.Purifying technique can be kept away the quartz of carrying secretly in the wilkinite, calcite, the negative impact that impurity such as feldspar cause the later stage building-up reactions.Purifying technique is by the washing among Fig. 1, natural subsidence, removal of impurities, dry, pulverized for five steps and realize, wherein wash the dilute slurry that requirement is mixed with grinding particle size 120 orders-200 purpose bentonite origin breeze, the bentonite particle diameter of pulverizing after requiring to purify reaches 120 orders-200 order.To handle be that bentonite through purifying after and caustic soda (sodium hydroxide) are pressed mass ratio 1: 1-1 to the alkali fusion activating process among Fig. 1: 1.6 prepare burden, and mix afterwards in 300 ℃-600 ℃ retort furnace roasting 1-6 hour, promptly obtain Powdered activation grog.Grog among Fig. 1 after the alkali fusion activation is through pulverizing, and granularity requirements is 120 orders-200 orders.Water dissolution-mode transfer among Fig. 1-reaction aging technique is that water is pressed Al with grog and aluminium hydroxide after the activation of alkali fusion activating process 2O 3: SiO 2: Na 2O: H 2O :=1: (1.8-2.3): (2.9-3.2): (170-220) feed intake (according to the activation degree of bentonite), under 40 ℃-100 ℃ aging temperature, wear out 2-8 hour to obtaining original liquid.Crystallization process is the crystal seed that original liquid after handling through purification-alkali fusion activation-water dissolution-mode transfer-reaction aging technique drops into 0.5%-7% among Fig. 1, under 60 ℃-120 ℃ temperature crystallization 5-24 hour, promptly gets the product feed liquid.Product feed liquid after will-crystallization process aging through purification-alkali fusion activation-water dissolution-mode transfer-reaction among Fig. 1 handling is carried out solid-liquid separation, and liquid phase is delivered to water dissolution-mode transfer-reaction aging technique section and is used to adjust Al 2O 3, SiO 2, Na 2O, H 2The mol ratio of O, solid phase are P type washing zeolite.Gained solid phase after will-crystallization-solid-liquid separation aging through purification-alkali fusion activation-water dissolution-mode transfer-reaction among Fig. 1 is washed, and wash water is delivered to water dissolution-mode transfer-reaction aging technique section and is used to adjust Al 2O 3, SiO 2, Na 2O, H 2The mol ratio of O, the filter cake drying, pulverization process promptly obtains P type washing zeolite product.
The specific embodiment of the present invention
Embodiment 1:
1, purify: with the dilute slurry that 120 purpose bentonites are mixed with, through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 120 orders, the bentonite after obtaining purifying.
2, alkali fusion activation: bentonite 20g after 1 processing of learning from else's experience and caustic soda (sodium hydroxide) 20g mix back roasting in 600 ℃ retort furnace and reacted 1 hour, promptly obtain Powdered activation back grog.
3, hydrolysis-mode transfer-reaction is aging: will be through grog and the aluminium hydroxide after 2 processing, and water is pressed Al 2O 3: SiO 2: Na 2O: H 2O=1: feed intake at 1.8: 2.9: 170, reaction is 2 hours under 40 ℃ aging temperature, makes original liquid.
4, crystallization: drop into 0.5% crystal seed in the original liquid that step 3 obtains, crystallization is 5 hours under 60 ℃ temperature, promptly gets the product feed liquid.
5, solid-liquid separation: the product feed liquid is carried out solid-liquid separation, and liquid phase is circulated to step 3 and is used for the mode transfer processing, and solid phase is P type washing zeolite.
6, solid phase is handled: to PH=7, filtrate cycle to step 3 is used for mode transfer to be handled the solid phase that step 5 is obtained through deionized water wash, and the filter cake drying makes P type washing zeolite product after the pulverizing.
Product sample (Sample1) calcium ion-exchanged performance such as table 1 with above-mentioned gained.
Embodiment 2:
1, purify: with the dilute slurry that 120 purpose bentonites are mixed with, through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 120 orders, the bentonite after obtaining purifying.
2, alkali fusion activation: bentonite 20g after 1 processing of learning from else's experience and caustic soda (sodium hydroxide) 22g mix back roasting in 300 ℃ retort furnace and reacted 6 hours, promptly obtain Powdered activation back grog.
3, hydrolysis-mode transfer-reaction is aging: will be through grog and the aluminium hydroxide after 2 processing, and water is pressed Al 2O 3: SiO 2: Na 2O: H 2O=1: feed intake at 2: 3.1: 200, reaction is 5 hours under 40 ℃ aging temperature, makes original liquid.
4, crystallization: drop into 6% crystal seed in the original liquid that step 3 obtains, crystallization is 12 hours under 90 ℃ temperature, promptly gets the product feed liquid.
5, solid-liquid separation: the product feed liquid is carried out solid-liquid separation, and liquid phase is circulated to step 3 and is used for the mode transfer processing, and solid phase is P type washing zeolite.
6, solid phase is handled: to PH=7, filtrate cycle to step 3 is used for mode transfer to be handled the solid phase that step 5 is obtained through deionized water wash, and the filter cake drying makes P type washing zeolite product after the pulverizing.
Product sample (Sample2) the calcium ion-exchanged performance of above-mentioned gained is listed in the table 1.
Embodiment 3:
1, purify: with the dilute slurry that 120 purpose bentonites are mixed with, through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 120 orders, the bentonite after obtaining purifying.
2, alkali fusion activation: bentonite 20g after 1 processing of learning from else's experience and caustic soda (sodium hydroxide) 24g mix back roasting in 350 ℃ retort furnace and reacted 3 hours, promptly obtain Powdered activation back grog.
3, hydrolysis-mode transfer-reaction is aging: will be through grog and the aluminium hydroxide after 2 processing, and water is pressed Al 2O 3: SiO 2: Na 2O: H 2O=1: feed intake at 2.3: 3.2: 220, reaction is 8 hours under 40 ℃ aging temperature, makes original liquid.
4, crystallization: drop into 2% crystal seed in the original liquid that step 3 obtains, crystallization is 24 hours under 120 ℃ temperature, promptly gets the product feed liquid.
5, solid-liquid separation: the product feed liquid is carried out solid-liquid separation, and liquid phase is circulated to step 3 and is used for the mode transfer processing, and solid phase is P type washing zeolite.
6, solid phase is handled: to PH=7, filtrate cycle to step 3 is used for mode transfer to be handled the solid phase that step 5 is obtained through deionized water wash, and the filter cake drying makes P type washing zeolite product after the pulverizing.
Above-mentioned product sample (Sample3) the calcium ion-exchanged performance that gets is listed in the table 1.
Embodiment 4:
1, purify: with the dilute slurry that 150 purpose bentonites are mixed with, through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 150 orders, the bentonite after obtaining purifying.
2, alkali fusion activation: bentonite 20g after 1 processing of learning from else's experience and caustic soda (sodium hydroxide) 32g mix back roasting in 350 ℃ retort furnace and reacted 5 hours, promptly obtain Powdered activation back grog.
3, hydrolysis-mode transfer-reaction is aging: will be through grog and the aluminium hydroxide after 2 processing, and water is pressed Al 2O 3: SiO 2: Na 2O: H 2O=1: feed intake at 2.3: 3.0: 200, reaction is 2 hours under 40 ℃ aging temperature, makes original liquid.
4, crystallization: drop into 4% crystal seed in the original liquid that step 3 obtains, crystallization is 2 hours under 75 ℃ temperature, promptly gets the product feed liquid.
5, solid-liquid separation: the product feed liquid is carried out solid-liquid separation, and liquid phase is circulated to step 3 and is used for the mode transfer processing, and solid phase is P type washing zeolite.
6, solid phase is handled: to PH=8, filtrate cycle to step 3 is used for mode transfer to be handled the solid phase that step 5 is obtained through deionized water wash, and the filter cake drying makes P type washing zeolite product after the pulverizing.
Product sample (Sample4) the calcium ion-exchanged performance of above-mentioned gained is listed in the table 1.
Embodiment 5:
1, purify: with the dilute slurry that 170 purpose bentonites are mixed with, through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 170 orders, the bentonite after obtaining purifying.
2, alkali fusion activation: bentonite 40g caustic soda (sodium hydroxide) 48g after 1 processing of learning from else's experience mixes back roasting in 400 ℃ retort furnace and reacted 4 hours, promptly obtains Powdered activation back grog.
3, water dissolution-mode transfer-reaction is aging: will be through grog and the aluminium hydroxide after 2 processing, and water is pressed Al 2O 3: SiO 2: Na 2O: H 2O=1: feed intake at 2.1: 3.0: 190, reaction is 5 hours under 75 ℃ aging temperature, makes original liquid.
4, crystallization: drop into 1% crystal seed in the original liquid that step 3 obtains, crystallization is 24 hours under 110 ℃ temperature, promptly gets the product feed liquid.
5, solid-liquid separation: the product feed liquid is carried out solid-liquid separation, and liquid phase is circulated to step 3 and is used for the mode transfer processing, and solid phase is P type washing zeolite.
6, solid phase is handled: to PH=8, filtrate cycle to step 3 is used for mode transfer to be handled the solid phase that step 5 is obtained through deionized water wash, and the filter cake drying makes P type washing zeolite product after the pulverizing.
Product sample (Sample5) the calcium ion-exchanged performance of above-mentioned gained is listed in the table 1.
Embodiment 6:
1, purify: with the dilute slurry that 200 purpose bentonites are mixed with, through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 200 orders, the bentonite after obtaining purifying.
2, alkali fusion activation: bentonite 40g after 1 processing of learning from else's experience and caustic soda (sodium hydroxide) 50g mix back roasting in 450 ℃ retort furnace and reacted 3 hours, promptly obtain Powdered activation back grog.
3, hydrolysis-mode transfer-reaction is aging: will be through grog and the aluminium hydroxide after 2 processing, and water is pressed Al 2O 3: SiO 2: Na 2O: H 2O=1: feed intake at 2: 3.2: 180, reaction is 8 hours under 75 ℃ aging temperature, makes original liquid.
4, crystallization: drop into 5% crystal seed in the original liquid that step 3 obtains, crystallization is 5 hours under 120 ℃ temperature, promptly gets the product feed liquid.
4, solid-liquid separation: the product feed liquid is carried out solid-liquid separation, and liquid phase is circulated to step 3 and is used for the mode transfer processing, and solid phase is P type washing zeolite.
6, solid phase is handled: to PH=8, filtrate cycle to step 3 is used for mode transfer to be handled the solid phase that step 5 is obtained through deionized water wash, and the filter cake drying makes P type washing zeolite product after the pulverizing.
Product sample (Sample6) the calcium ion-exchanged performance of above-mentioned gained is listed in the table 1.
Embodiment 7:
1, purify: with the dilute slurry that 170 purpose bentonites are mixed with, through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 170 orders, the bentonite after obtaining purifying.
5, alkali fusion activation: bentonite 50g after 1 processing of learning from else's experience and caustic soda (sodium hydroxide) 65g mix back roasting in 500 ℃ retort furnace and reacted 2 hours, promptly obtain Powdered activation back grog.
3, hydrolysis-mode transfer-reaction is aging: will be through grog and the aluminium hydroxide after 2 processing, and water is pressed Al 2O 3: SiO 2: Na 2O: H 2O=1: feed intake at 2.2: 3: 210, reaction is 2 hours under 100 ℃ aging temperature, makes original liquid.
4, crystallization: drop into 3% crystal seed in the original liquid that step 3 obtains, crystallization is 24 hours under 110 ℃ temperature, promptly gets the product feed liquid.
5, solid-liquid separation: the product feed liquid is carried out solid-liquid separation, and liquid phase is circulated to step 3 and is used for the mode transfer processing, and solid phase is P type washing zeolite.
6, solid phase is handled: to PH=7, filtrate cycle to step 3 is used for mode transfer to be handled the solid phase that step 5 is obtained through deionized water wash, and the filter cake drying makes P type washing zeolite product after the pulverizing.
Product sample (Sample7) the calcium ion-exchanged performance of above-mentioned gained is listed in the table 1.
Embodiment 8:
1, purify: with the dilute slurry that 150 purpose bentonites are mixed with, through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 150 orders, the bentonite after obtaining purifying.
2, alkali fusion activation: bentonite 30g after 1 processing of learning from else's experience and caustic soda (sodium hydroxide) 48g mix back roasting in 550 ℃ retort furnace and reacted 1 hour, promptly obtain Powdered activation back grog.
3, hydrolysis-mode transfer-reaction is aging: will be through grog and the aluminium hydroxide after 2 processing, and water is pressed Al 2O 3: SiO 2: Na 2O: H 2O=1: feed intake at 1.8: 3.2: 220, reaction is 2 hours under 100 ℃ aging temperature, makes original liquid.
4, crystallization: drop into 5% crystal seed in the original liquid that step 3 obtains, crystallization is 5 hours under 120 ℃ temperature, promptly gets the product feed liquid.
5, solid-liquid separation: the product feed liquid is carried out solid-liquid separation, and liquid phase is circulated to step 3 and is used for the mode transfer processing, and solid phase is P type washing zeolite.
6, solid phase is handled: to PH=8, filtrate cycle to step 3 is used for mode transfer to be handled the solid phase that step 5 is obtained through deionized water wash, and the filter cake drying makes P type washing zeolite product after the pulverizing.
Product sample (Sample8) the calcium ion-exchanged performance of above-mentioned gained is listed in the table 1.
Embodiment 9:
1, purify: with the dilute slurry that 120 purpose bentonites are mixed with, through natural subsidence, except that behind the sub-cloud impurity, oven dry is crushed to 120 orders, the bentonite after obtaining purifying.
2, alkali fusion activation: bentonite 40g after 1 processing of learning from else's experience and caustic soda (sodium hydroxide) 40g mix back roasting in 600 ℃ retort furnace and reacted 2 hours, promptly obtain Powdered activation back grog.
3. hydrolysis-mode transfer-reaction is aging: will be through grog and the aluminium hydroxide after 2 processing, and water is pressed Al 2O 3: SiO 2: Na 2O: H 2O=1: feed intake at 2.3: 3.1: 220, reaction is 8 hours under 100 ℃ aging temperature, makes original liquid.
4, crystallization: drop into 7% crystal seed in the original liquid that step 3 obtains, crystallization is 12 hours under 120 ℃ temperature, promptly gets the product feed liquid.
5, solid-liquid separation: the product feed liquid is carried out solid-liquid separation, and liquid phase is circulated to step 3 and is used for the mode transfer processing, and solid phase is P type washing zeolite.
6, solid phase is handled: to PH=7, filtrate cycle to step 3 is used for mode transfer to be handled the solid phase that step 5 is obtained through deionized water wash, and the filter cake drying makes P type washing zeolite product after the pulverizing.
To list in the table 1 through product sample (Sample9) the calcium ion-exchanged performance of above-mentioned gained.
Over-all properties with the inventive method synthetic P washing zeolite is measured as table 2.
Each embodiment of table 1 obtains the calcium ion exchange capacity guide look of P type washing zeolite
Embodiment ????1 ????2 ????3 ????4 ????5 ????6 ????7 ????8 ????9
Exchange capacity (the mgCaCO of calcium 3The anhydrous P type of/g zeolite) ???326 ???343 ???318 ???341 ???325 ???361 ???358 ???317 ???332
Table 2 synthetic P of the present invention type washing zeolite over-all properties measurement result
Performance Calcium ion-exchanged (mgCaCO 3The anhydrous P type of/g zeolite) Granularity (%) Whiteness (W=Y) PH value (1% solution, 25 ℃) Loss on ignition (800 ± 10 ℃, 3h) %
??≤10μm ??≤4μm
P type zeolite product ????330 ??≥99 ??≥94 ????96 ????8.5 ????19.85

Claims (7)

1, a kind of alkaline process activated bentonite is produced the processing method of P type washing zeolite, and it is characterized in that: its processing step is as follows:
(1) purify: bentonite is washed, removal of impurities, oven dry, standby after the pulverization process;
(2) alkali fusion activation: will after wilkinite after the pulverization process and caustic soda (sodium hydroxide) pressed powder mix, carry out the processing of alkali fusion activating process;
(3) water dissolution-mode transfer-reaction is aging: the activation raw material after the alkali fusion activating process is handled is adjusted Al through water dissolution 2O 3, SiO 2, Na 2O, H 2The mol ratio of O is reacted burin-in process after being suitable proportion;
(4) crystallization: will carry out the crystallization processing through the feed liquid of reacting after wearing out;
(5) solid-liquid separation: feed liquid that will be after crystallization, carry out solid-liquid separation, liquid phase is delivered to water dissolution-mode transfer-reaction aging technique section and is used to adjust Al 2O 3, SiO 2, Na 2O, H 2The mol ratio of O, solid phase are P type washing zeolite;
(6) solid phase is handled: will be after solid-liquid separation the gained solid phase, wash, wash water is delivered to water dissolution-mode transfer-reaction aging technique section and is used to adjust Al 2O 3, SiO 2, Na 2O, H 2The mol ratio of O, the filter cake drying, pulverization process promptly obtains P type washing zeolite product.
2, the processing method of producing P type washing zeolite according to the said alkaline process activated bentonite of claim 1, it is characterized in that: the grinding particle size of described bentonite before washing is 120 orders-200 orders.
3, the processing method of producing P type washing zeolite according to the said alkaline process activated bentonite of claim 1, it is characterized in that: it is the dilute slurry that grinding particle size 120 orders-200 purpose bentonite is mixed with that purifying technique is handled, through natural subsidence, after removing sub-cloud impurity, oven dry is crushed to 120 orders-200 order and promptly gets the back bentonite of purifying.
4, the processing method of producing P type washing zeolite according to the said alkaline process activated bentonite of claim 1, it is characterized in that: the alkali fusion activating process is that bentonite after purifying and caustic soda (sodium hydroxide) are pressed mass ratio 1: 1-1: 1.6 batchings, mix the back and in 300 ℃-600 ℃ retort furnace, reacted 1-6 hour, promptly obtain Powdered activation back grog.
5, produce the processing method of P type washing zeolite according to the said alkaline process activated bentonite of claim 1, it is characterized in that: water dissolution-mode transfer-reaction aging technique is with the grog after activating through the alkali fusion activating process and aluminium hydroxide, water, presses Al 2O 3: SiO 2: Na 2O: H 2O :=1: (1.8-2.3): (2.9-3.2): (170-220) feed intake after, under 40 ℃-100 ℃ aging temperature aging 2-8 hour, promptly get the original liquid for preparing P type washing zeolite.
6, the processing method of producing P type washing zeolite according to the said alkaline process activated bentonite of claim 1, it is characterized in that: crystallization process is the crystal seed that the original liquid after handling through the reaction aging technique drops into 0.5%-7%, under 60 ℃-120 ℃ temperature crystallization 5-24 hour, promptly get the product feed liquid.
7, the processing method of producing P type washing zeolite according to the said alkaline process activated bentonite of claim 1, it is characterized in that: solid-liquid separation, the solid phase of gained to PH=7-8, promptly obtain filter cake through deionized water wash, the filter cake drying promptly gets P type washing zeolite product after the pulverizing.
CNB021564825A 2002-12-18 2002-12-18 Technical method for producing P type zeolite for washing use by activating bentonite with alkaline process being utilized Expired - Fee Related CN1162527C (en)

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CN103601210A (en) * 2013-12-03 2014-02-26 西南科技大学 Method for synthesizing zeolite by one-step alkali dissolution of bentonite
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1321891C (en) * 2005-09-22 2007-06-20 山东铝业股份有限公司 Method for preparing P type zeolite in sodium silicate-containing sodium aluminate solution
CN103274427A (en) * 2013-06-18 2013-09-04 北京北大先锋科技有限公司 Preparation method for P-shaped molecular sieve
CN103601210A (en) * 2013-12-03 2014-02-26 西南科技大学 Method for synthesizing zeolite by one-step alkali dissolution of bentonite
CN103601210B (en) * 2013-12-03 2015-08-05 西南科技大学 Wilkinite one step alkali is fused into the method for zeolite
CN106745058A (en) * 2016-12-28 2017-05-31 河南大学 A kind of microwave preparation of p-type molecular sieve
CN106745058B (en) * 2016-12-28 2019-09-10 河南大学 A kind of microwave preparation of p-zeolite
CN108439424A (en) * 2018-04-30 2018-08-24 东北石油大学 The method that the cubic type zeolite of high absorption property is prepared using rice husk as raw material
CN108439424B (en) * 2018-04-30 2021-08-24 东北石油大学 Method for preparing cubic zeolite with high adsorption performance by using rice hulls as raw materials

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