CN100457620C - Process for preparing natural magnesium aluminium silicate gel - Google Patents
Process for preparing natural magnesium aluminium silicate gel Download PDFInfo
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- CN100457620C CN100457620C CNB02112616XA CN02112616A CN100457620C CN 100457620 C CN100457620 C CN 100457620C CN B02112616X A CNB02112616X A CN B02112616XA CN 02112616 A CN02112616 A CN 02112616A CN 100457620 C CN100457620 C CN 100457620C
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- ore pulp
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- mineral
- inorganic salt
- viscosity
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Abstract
A process for preparing natural gel of magnesium aluminium silicate from bentonite, attapulgite, bentone, etc includes such steps as pulverizing, preparing slurry, adding pour depressor, stirring, dynamic centrifugal separation, adding inorganic salt containing one-valence metal ions, stirring, pre-activating, adding organic salt containing at least Na ions, stirring for modifying, and post-treating.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic gel, the clay mineral that particularly a kind of employing contains the magnalium composition is the method for feedstock production natural magnesium aluminium silicate gel.
Background technology
Natural magnesium aluminium silicate gel be a kind of be raw material with the clay mineral that contains the magnalium composition, the mineral coagulant material of a kind of purifying modification that obtains by technological processs such as purification, purifying, modifications.This mineral coagulant material has surprising swelling capacity in water, can form the gel of card room shape structure, this gel has good thixotropy, i.e. retrogradation under static condition, be semi-solid state, but thinning under external force, have good flowability, be good viscosity modifier, thickening material, suspension agent, emulsion stabilizer, fluid thixotropy conditioning agent, be widely used in industries such as daily-use chemical industry, pharmacy, building materials, coating, oil drilling, rubber and precision casting.
In order to obtain this mineral coagulant material, 1989 the 4th phases " inorganic chemicals industry " magazine had once been delivered one piece, the article that is entitled as " development of XVT inorganic gel and application thereof " that Xinjiang chemical engineering design research institute Wang Daorong is write.It is the method that raw material is developed into XVT inorganic gel product with the smectite mineral that this article discloses a kind of.It is to the effect that: 1, the ore powder with the smectite mineral is broken to certain fineness (as 100～200 orders); 2, soak, smash slurry, disperse; 3, adopt natural sedimentation to remove non-dispersive impurity,, ore pulp is purified as rhombspar, quartzite, calcite etc.; 4, again leaching gained ore pulp is concentrated; 5, to the ore pulp after concentrating with containing Na
+Inorganic salt carry out modification, to improve colloidal property; 6, the colloid material after the modification is dried, obtain the white plates gel product at last.
Although above-mentioned achievement is obtaining first-stage success aspect the preparation technology who explores natural magnesium aluminium silicate gel, but from angle of practical application, still there is following defective: 1, owing to the 3rd step adopted natural sedimentation (or gravity method) under static state the mineral grain in the ore pulp to be purified, operation concentration has been subjected to strict restriction, in other words pulp density need be lower than solid-to-liquid ratio 1: 10, be that concentration expressed in percentage by weight need be lower than 9%, otherwise ore pulp can be very poor because of excessive concentration, the excessive refining effect that causes of viscosity.And the natural sedimentation purification process is slow, generally needs 14～16 hours, and production efficiency is extremely low.2, in second step, if use viscosity-depression agent then can cause the viscosity of the finished product and colloidal property to decline to a great extent, if do not use viscosity-depression agent can cause ore pulp poor because of dispersion effect yet, reduce the purification separating effect greatly, thereby in the mineral purification process, dare not use viscosity-depression agent or strict control consumption, and cause the ore pulp degree of scatter not enough, caused refining effect poor equally, purpose mineral purification degrees is low in the product, therefore directly influences the range of application of product.3, because the mineral purification degrees is low, add that modified technique is simple, make that final gel product is second-rate, the gel viscosity of its 5% aqueous dispersions had only for 40～60 milli handkerchief seconds, and the thixotroping value only is 1.3～1.4, and the less stable of gel.For this reason, the present invention is from improving the angle of processing method, created a kind of preparation method of new natural magnesium aluminium silicate gel, to overcome the deficiencies in the prior art.
Summary of the invention
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of natural magnesium aluminium silicate gel is a raw material with the natural magnesium aluminium silicate mineral, follows these steps to be prepared:
(1), raw material is pulverized;
(2), the breeze after will pulverizing adds water and makes ore pulp, and adds viscosity-depression agent and fully stirs, and mineral grain is dispersed in the ore pulp;
(3), adopt the dynamic separation method of purification of centrifuge field, ore pulp is separated purification;
(4), add in the ore pulp after purification and contain the inorganic salt of monovalent metallic ion, and fully stir, gelling property is carried out preactivate handles;
(5), adding contains Na at least in the ore pulp that preactivate is handled
+Inorganic salt as properties-correcting agent, and fully stir, the natural magnesium aluminium silicate mineral in the ore pulp are carried out modification;
(6), the ore pulp after the modification is carried out aftertreatment, thus obtain the finished product.
In the technique scheme, described raw material can adopt bentonite, smectite, attapulgite, wilkinite etc. to contain the mineral of natural magnesium aluminium silicate.
In the above-mentioned the first step, raw material pulverized preferably adopt the iron-free medium, the smashing fineness of ore is 100～325 orders.
In above-mentioned second step, the solid-to-liquid ratio that breeze is added water slurrying is 1: 10～1: 1.8, and promptly weight percent concentration is 9%～36% ore pulp, and preferable solid-to-liquid ratio scope is 1: 4～1: 2.3, and promptly weight percent concentration is 20%～30% ore pulp.Need smash slurry (stirring) to ore pulp during slurrying, smash 30～60 minutes slurry time.Smash in the slurry process and add viscosity-depression agent, as Sodium hexametaphosphate 99, trisodium phosphate, tannic acid, sodium polyacrylate etc., its consumption is 0.1～15% of the contained dried ore deposit of ore pulp, and preferable consumption is 0.5～10% of the contained dried ore deposit of ore pulp.Under the acting in conjunction of mechanical stirring power and hydrodynamic shear, the natural magnesium aluminium silicate mineral in the ore are dispersed in the ore pulp with the form of small mineral grain in this step.Here it should be noted that and disperse to be meant that mineral totally are evenly distributed in the ore pulp with the form of molecule, rather than be dispersed in the ore pulp, do not exist but also do not repel the mineral that a small amount of ionic condition is arranged in the ore pulp with the form of ionic condition.
In above-mentioned the 3rd step, described dynamic centrifugation is purified and is adopted the dynamic separation equipment for purifying with centrifuge field to carry out, as hydrocyclone, centrifugal classifier etc., make the content that separates useful purpose mineral in the ore pulp of purifying greater than 80%, pulp density is greater than 4% (concentration expressed in percentage by weight).
In above-mentioned the 4th step, described monovalent metallic ion comprises Li
+, H
+, Na
+, K
+, its inorganic salt such as Li
2SO
4, H
2SO
4, HCl, Na
2CO
3, NaCl, Na
2SO
4, KCl, K
2SO
4Deng.The inorganic salt of the monovalent metallic ion of described adding can be selected a kind of in the inorganic salt of above-mentioned monovalent metallic ion, and 2～4 kinds in also can the inorganic salt of above-mentioned monovalent metallic ion be mixed and use.The inorganic salt consumption of the monovalent metallic ion that adds by processing breeze weight 2～20%.In order more to help activating reaction, this reaction can be carried out in a reactor that has agitating function and a heating function, and suitable temperature of reaction is 10～90 ℃, and reaction pressure is a normal pressure, in 10～30 minutes reaction times, agitator speed can be at 1000～3000 rev/mins.
In above-mentioned the 5th step, described properties-correcting agent can select to contain Na separately
+Inorganic salt, also can select 1～3 kind and comprise Na
+Mix with the inorganic salt of the metal ion of different valence mumbers and to use, its add-on by processing breeze weight 2～20%.The metal ion of described different valence mumbers comprises Na
+, Mg
++, Fe
+++Or Al
+++This is reflected under the agitation condition, reacts 10～30 minutes, and suitable temperature of reaction is 10～90 ℃, is reflected under the normal pressure and carries out, and the pH value of its ore pulp of reaction end of a period should be between 5～9, preferably between 6～9.
In above-mentioned the 6th step, described aftertreatment is meant carries out processing such as drying, pulverizing, sterilization, packing to the gel ore pulp, wherein oven dry can adopt spray drying device to carry out drying, acquisition moisture is 5～10% white hollow granular product, also can adopt drum drying equipment carry out drying above-mentioned material, obtain water content and be 8～12% white plates product.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1, step 1 of the present invention has been because of having adopted iron-free medium disintegrating apparatus and technology, thereby can farthest avoid the irony in the abrasive dust course of processing to pollute, and can make the Fe of final gel product
2O
3Content is lower than 1.0%, and whiteness is greater than 75%, thereby has enlarged the Application Areas of this series products greatly.
2, in the step 2 of the present invention owing to used suitable viscosity-depression agent, thereby improved greatly and smash slurry operation concentration, can make and smash slurry operation concentration and be increased to 20～36%, improved the processing power (improving 2～3 times) of equipment greatly and, created good condition for separating to purify owing to strengthened the dispersiveness of ore pulp.
3, step 3 of the present invention is owing to the dynamic separation method of purification that has adopted in centrifuge field, eliminated the thixotropy that has had because of mineral itself and mineral have been separated the disadvantageous effect of purifying and producing, so the advantage of present method is the purification efficiency height, the purification degrees height of purpose mineral in the products obtained therefrom.Simultaneously, this purification separating technology can carry out continuously, and processing power is big, can realize scale operation, and can carry out automatization control to flow process.By this novel process to containing neusilin mineral (as bentonite, smectite, attapulgite, the swelling soil) separation of purifying, can obtain highly purified purifying mineral products (the natural magnesium aluminium silicate mineral purity is greater than 80%), and the purity of purpose mineral products can be regulated as required.
4, the 4th step of the present invention is the reaction of gelling preactivate, and this reaction adopts again the ore pulp gellifying property after the activated method is handled viscosity-depression agent to activate, thereby in mineral purification detached job, can courageously use viscosity-depression agent according to purification operation needs.
5, the present invention uses the metallic cation of different valence mumbers the 5th step, and the blended method has replaced original single Na by a certain percentage
+To the method for modifying of gelatinous material, make the viscosity of gel obtain bigger raising, stability is better.
6, after the present invention adopted spray drying process in the 6th step, products obtained therefrom is hollow thin round shaped grain shape, compares institute with sheet material and takes up space lessly, is convenient to the packing of product, can shorten simultaneously the gelation time of glue, compare with sheet material and can make gelation time shortening about 30%.
In sum, the technology of the present invention core is: the use of viscosity-depression agent and the inorganic salt modification of dynamically centrifugation purification, preactivate processing and different valence mumber metal ions are combined, both solved the contradiction of using between viscosity-depression agent and the gellifying property decline, found the method for activated gel performance again, solve the contradiction between pulp density and refining effect in the mineral purification process again, thereby obtained significant technique effect.
Description of drawings
Accompanying drawing 1 is process flow sheet of the present invention;
Accompanying drawing 2 is an embodiment of the invention process flow sheet.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
Embodiment: shown in accompanying drawing 2, a kind of preparation method of natural magnesium aluminium silicate gel is a raw material with natural smectite mineral, follows these steps to be prepared:
1, (major ingredient is MgO 7.0% CaO 13.70% Al with the smectite ore
2O
39.32% Fe
2O
32.64%) being broken to fineness through the iron-free medium powder is 100～200 purpose breezes.
2, this breeze is added water, be made into concentration expressed in percentage by weight and be 20～30% ore pulp, smash slurry, smash 40 minutes slurry time, in ore pulp, add when smashing slurry and account for the viscosity-depression agent Sodium hexametaphosphate 99 of doing ore deposit weight 0.5～10%.
3, smash slurry operation gained ore pulp through the sorting of secondary hydrocyclone, give ore deposit pressure 0.1～0.5Mpa (MPa), gained overflow ore pulp is the separation of purifying under 600～2000 the condition at separation factor with centrifugal classifier again, and obtaining concentration is 4%～5% purification ore pulp.In this ore pulp, smectite content is greater than 80%, and its major ingredient is MgO 18～24% CaO 5～8% Al
2O
33.5～5.0% Fe
2O
31.0～0.6%.
4, above-mentioned purification ore pulp is injected in the reactor of a belt stirrer, in whipped state downhill reaction device, slowly add the A medicament that accounts for mineral weight (amount to and become to do the ore deposit meter) 2～15%.The A medicament is by Li
2SO
4, K
2SO
4And H
2SO
4In 1: (0.8～5): the ratio preparation of (0.5～5).Be reflected under the normal pressure and carry out, 10～80 ℃ of temperature of reaction, 10～30 minutes reaction times.
5, after above-mentioned reaction finishes, in this reactor, add properties-correcting agent B again, its consumption for processing breeze weight (amount to become to do the ore deposit count) 2～20%.The B medicament is by Na
2CO
3, MgSO
4And Al
2(SO
4)
3By 1: (0.2～5): the mixed of (0.2～4) forms.10～30 minutes reaction times, 10～80 ℃ of temperature of reaction.
6, carry out drying by the 5th step gained paste shape material with spray drying device, 120 ℃～300 ℃ of drying temperatures, obtaining particle diameter is that 60～150 orders, water content are 8～10% powder-like product, product whiteness is greater than 75%.
7, pass through the product of 1～6 step process gained, it is carried out glue, at the homogenizer rotating speed is 3000 rev/mins, and 25 ℃ of slurry temperatures stirred 40 minutes, gel strength 5% (aqueous dispersions), availability is stable, and viscosity number was 100～500 milli handkerchief seconds, and the thixotroping value is 1.4～1.6 high quality inorganic gel, and original its viscosity number of technology gained like product only was 40～60 milli handkerchief seconds, and the thixotroping value only is 1.3～1.4.
Claims (10)
1, a kind of preparation method of natural magnesium aluminium silicate gel is characterized in that: with the natural magnesium aluminium silicate mineral is raw material, follows these steps to be prepared:
(1), raw material is pulverized;
(2), the breeze after will pulverizing adds water and makes ore pulp, and adds viscosity-depression agent and fully stirs, and mineral grain is dispersed in the ore pulp;
(3), adopt the dynamic separation method of purification of centrifuge field, ore pulp is separated purification;
(4), add in the ore pulp after purification and contain the inorganic salt of monovalent metallic ion, and fully stir, gelling property is carried out preactivate handles;
(5), adding contains Na at least in the ore pulp that preactivate is handled
+Inorganic salt as properties-correcting agent, and fully stir, the natural magnesium aluminium silicate mineral in the ore pulp are carried out modification;
(6), the ore pulp after the modification is carried out aftertreatment, thus obtain the finished product.
2, preparation method according to claim 1 is characterized in that: described raw material adopts smectite, bentonite, wilkinite or attapulgite mineral.
3, preparation method according to claim 1 is characterized in that: in the above-mentioned the first step, adopt the iron-free medium to pulverize to raw material.
4, preparation method according to claim 1 is characterized in that: in above-mentioned second step, the solid-to-liquid ratio of described ore pulp is 1: 10～1: 1.8, and promptly weight percent concentration is 9%～36% ore pulp; The consumption of viscosity-depression agent is 0.1～15% of the contained dried ore deposit of ore pulp.
5, preparation method according to claim 4 is characterized in that: described solid-to-liquid ratio is 1: 4～1: 2.3, and promptly weight percent concentration is 20%～30% ore pulp; The consumption of viscosity-depression agent is 0.5～10% of the contained dried ore deposit of ore pulp.
6, preparation method according to claim 5 is characterized in that: described viscosity-depression agent is Sodium hexametaphosphate 99, trisodium phosphate, tannic acid or sodium polyacrylate.
7, preparation method according to claim 1 is characterized in that: in above-mentioned the 4th step, described monovalent metallic ion comprises Li
+, H
+, Na
+And K
+The inorganic salt consumption of the monovalent metallic ion that adds by processing breeze weight 2～20%.
8, preparation method according to claim 7 is characterized in that: the inorganic salt of described monovalent metallic ion are selected Li
2SO
4, H
2SO
4, HCl, Na
2CO
3, NaCl, Na
2SO
4, KCl, K
2SO
4In 2～4 kinds mix to use.
9, preparation method according to claim 1 is characterized in that: in above-mentioned the 5th step, described properties-correcting agent selects the inorganic salt of the metal ion of different valence mumbers mix to use, add-on by processing breeze weight 2～20%.
10, preparation method according to claim 9 is characterized in that: the metal ion of described different valence mumbers comprises Na
+, Mg
++, Fe
+++And Al
+++
Priority Applications (1)
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|---|---|---|---|
| CNB02112616XA CN100457620C (en) | 2002-01-28 | 2002-01-28 | Process for preparing natural magnesium aluminium silicate gel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02112616XA CN100457620C (en) | 2002-01-28 | 2002-01-28 | Process for preparing natural magnesium aluminium silicate gel |
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| CN1363515A CN1363515A (en) | 2002-08-14 |
| CN100457620C true CN100457620C (en) | 2009-02-04 |
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| CN1315726C (en) * | 2004-06-18 | 2007-05-16 | 中国建筑材料科学研究院 | Hydrated magnesium silicate and synthesis method thereof |
| CN1317067C (en) * | 2005-06-20 | 2007-05-23 | 许庆华 | Process for improving viscosity of attapulgite clay |
| CN1323941C (en) * | 2005-07-23 | 2007-07-04 | 桂林矿产地质研究院 | Modified bentonite used for treating garbage percolate and its manufacturing method |
| CN100443159C (en) * | 2006-06-15 | 2008-12-17 | 兰州大学 | Cation flocculant of surface modified attapulgite, and preparation method |
| CN102649572A (en) * | 2011-02-24 | 2012-08-29 | 中国科学院兰州化学物理研究所 | Preparation method for attapulgite clay inorganic gel |
| CN102786245B (en) * | 2012-07-23 | 2013-12-04 | 黑旋风工程机械开发有限公司 | Formula for viscosity reducer |
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| CN112007607A (en) * | 2020-05-15 | 2020-12-01 | 苏州国建慧投矿物新材料有限公司 | Bentonite mineral gel for water treatment and its preparation method |
| CN111825099A (en) * | 2020-09-09 | 2020-10-27 | 苏州国建慧投矿物新材料有限公司 | Aluminum magnesium silicate inorganic gel and preparation method thereof |
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-
2002
- 2002-01-28 CN CNB02112616XA patent/CN100457620C/en not_active Expired - Fee Related
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|---|---|---|---|---|
| CN1045081A (en) * | 1989-02-23 | 1990-09-05 | 太原工业大学 | High silicon crystalline aluminosilicate and derivative thereof is synthetic in the non-aqueous system |
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