CN1562745A - Method for preparing inorganic gel of aluminium magnesium silicate in high purity - Google Patents
Method for preparing inorganic gel of aluminium magnesium silicate in high purity Download PDFInfo
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- CN1562745A CN1562745A CN 200410039840 CN200410039840A CN1562745A CN 1562745 A CN1562745 A CN 1562745A CN 200410039840 CN200410039840 CN 200410039840 CN 200410039840 A CN200410039840 A CN 200410039840A CN 1562745 A CN1562745 A CN 1562745A
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- ore pulp
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- magnetic separator
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Abstract
The the invention, magnesium lithium soapstone, alta-mud, bentonite, concave-convex bar stone are used as raw material. The prepn. steps are in following: 1. mineral raw material crushing; 2. mixing mineral powder with water added viscosity reduce agent and pulping; 3. centrifuging and refining; 4. getting rid of iron by strong magnetic separator; 5. modifying by adding A-type modifier; 6 modifying by adding B-type modifier; 7 concentrating by centrifuger; 8 filtering and washing the ore pulp by alcohol agent; 9 drying the washed ore pulp to get product. the main techonlogy chracteristis are getting rid of iron by strong magnetic separator and washing by alcohol agent. The product is good thickener, suspending agent, viscosity regulator and thixotropy regulator.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic gel, particularly a kind of is the preparation method of the high purity silicic acid magnalium inorganic gel of raw material with the clay mineral that contains the neusilin composition.
Background technology
Aluminium magnesium silicate inorganic gel be a kind of be raw material with the clay mineral that contains the neusilin composition such as magnesium hectorite, wilkinite, bentonite, attapulgite etc., through technical process such as immersion, slurrying, purification, modification, washings, and the highly purified natural inorganic gelatinous material that obtains.The inorganic gel material of the octahedral layer frame shape structure that this inner tool is special has surprising swelling capacity in water, form gelinite with water, have good suspension, colloidal stability and thixotropy (promptly the thinning good fluidity of colloid, the static condition retrogradation is semi-solid performance) under external force.Be excellent viscosity conditioning agent, thickening material, suspension agent, stablizer, fluid thixotropy conditioning agent, be widely used in industries such as chemical industry, building materials, oil drilling, casting, its high purity product, field and prospect have a wide range of applications in industry such as medicine, food.
In order to obtain inorganic gel material with this mineral preparation, 1989 the 4th phases " inorganic chemicals industry " had once been delivered one piece, it is the method for feedstock production XVT inorganic gel with smectite (being the magnesium hectorite) mineral that 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, this article disclose a kind of.State Intellectual Property Office discloses the patent application of a kind of " preparation method of natural magnesium aluminium silicate gel " in the recent period, and application number is 02112616.X, and publication number is the invention of CN1363515A.This invention is to the effect that: the breeze that 1, raw material is crushed to certain fineness (100 orders-325 order); 2, the breeze after will pulverizing adds water and makes ore pulp, and adds viscosity-depression agent (Sodium hexametaphosphate 99 etc.) and carry out abundant dispersed with stirring; 3, adopt centrifugal separation method that ore pulp is purified; 4, add the inorganic salt mixt that contains monovalent metallic ion in the ore pulp after purification, gelling property is carried out preactivate handle; 5, adding contains Na at least in the ore pulp that preactivate is handled
+Inorganic salt as properties-correcting agent, ore pulp mesosilicic acid magnalium mineral are carried out modification; 6, the ore pulp after the modification is carried out aftertreatment, thereby obtain the finished product.Foregoing invention is obtaining certain effect aspect the preparation of aluminium magnesium silicate inorganic gel and the purification, but from practical application with improve the quality and still have following defective: 1, irony the product and irony oxide compound thereof, though the measure of adopting " iron-free medium " that mineral are pulverized is arranged as far as possible, but impurity such as the iron content of mining, transportation and ore itself and irony oxide compound still are difficult to be exempted from, fail effectively to remove, influenced the whiteness and the purity of product; 2, in preparation process, viscosity-depression agents such as Sodium hexametaphosphate 99 contain Li
+, Na
+, K
+, H
+Deng alkaline metal salt, excessive properties-correcting agent and by product, and other solubility salts in the process water etc. remain in the ore pulp solution, all enter product after the drying and crushing of ore pulp, cause purity, whiteness and quality product to be adversely affected; Cause product purity only below 97% by above-mentioned defective, can not satisfy fields such as medicine, food and will reach requirement more than 99%, limited of the application of this product in fields such as medicine, food to product purity.For this reason, the present invention has increased the step of two methods of purification on the basis of prior art processes flow process, has created a kind of preparation method of new aluminium magnesium silicate inorganic gel, to overcome the deficiencies in the prior art.
Summary of the invention
In order to achieve the above object, the step of technical scheme of the present invention has:
1, raw mineral materials is pulverized, fineness reaches the 100-325 order;
2, the breeze after will pulverizing adds water and makes the ore pulp that concentration is 10-40%, and adds viscosity-depression agent and fully stir, and makes its homodisperse.Described viscosity-depression agent is Sodium hexametaphosphate 99, trisodium phosphate, red phosphoric acid etc., and its consumption is the 0.2-12% of ore pulp solid content;
3, adopt continuously centrifuged to separate equipment for purifying, remove impurity such as grit as purifications such as hydrocyclones.Its centrifugation equipment for purifying can be one, also can be that many series connection are used;
4, add A type properties-correcting agent in the ore pulp after purification and carry out the chemical modification first time.A type properties-correcting agent is Li
2SO
4And K
2SO
4, both weight ratios are 1: (0.5-10), dosage is the 2-12% of ore pulp solid content, and pH value is controlled at 5-5.5, and temperature of reaction is 30-95 ℃, and the reaction times is 20-50 minute;
5, modification for the second time adds Type B properties-correcting agent MgSO
4And Al
2(SO
4)
3, the two weight ratio is 1: (1-1.5), dosage is the 1-1.5% of ore pulp solid content, the control pH value is that 8-9 (uses Na
2CO
3Regulate pH value), temperature of reaction is 30-60 ℃, the reaction times is 10-20 minute;
6, the ore pulp after twice modification concentrates through the continuous operating whizzer, and the continuous operating whizzer can be that unit concentrates, and also can be that multimachine concentrates, and also can carry out classification and concentrated simultaneously;
7, the gel ore pulp of finishing final modification and purification processes is carried out aftertreatment, comprising: drying, pulverizing, packing etc. finally obtain the aluminium magnesium silicate inorganic gel product.
In the technique scheme, described neusilin raw mineral materials can be: magnesium hectorite, wilkinite, bentonite or attapulgite.
Its feature part is also to comprise the following steps:
(1) adopt the Wet-type strong magnetic separator deironing, device is at technical scheme the 3rd step centrifugation equipment for purifying, after the ore pulp purification;
(2) the concentrated ore pulp after adopting alcohol agent to the purification modification carries out the washing of filter formula, and filter formula washing device is placed on after the 6th step of technical scheme ore pulp concentrates.
In (1) step that technique scheme feature part comprises, the magneticstrength of described Wet-type strong magnetic separator is 10000-25000 Gauss; Preferable magnetic field range is 18000-20000 Gauss.
In (2) step that technique scheme feature part comprises, described alcohol agent comprises methyl alcohol, ethanol, Virahol, can select for use wherein any; The add-on of alcohol agent is 1.5-3.0 a times of ore pulp solid content.Alcohol formulations in the filter formula washing rear filtrate reclaims by distillation method, is reused for washing next time, recycles.
Because the application of technique scheme, the present invention compared with prior art has following advantage:
1, owing to adopted the Wet-type strong magnetic separator deironing, can remove the 40-50% of iron and oxide impurity content thereof effectively, improve the whiteness and the purity of product.
2, owing to adopted alcohol agent to carry out carrying out washing treatment, further improved the purity of product, removed effectively and remained in the solubility salt that concentrates in the ore pulp of back.(comprising inorganic salt in the dispersion agent of adding, excessive properties-correcting agent, modification by product, the service water etc.).The filtrate that contains alcohol formulations is reclaimed with distillation method again, and its alcohol formulations of retrieving can recycle, and the washing of alcohol formulations also is disinfecting gel product.
In sum, owing to adopted the intensity magnetic separator deironing and adopted alcohol agent to wash, the purity of this inorganic gel product is reached more than 99%, whiteness reaches more than 75%, product is handled through pure wash disinfection and is more met hygienic requirements, widened application, thereby obtained significant technique effect in fields such as medicine and food.
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 specifically:
Embodiment: see shown in the accompanying drawing 2 that a kind of preparation method of high purity silicic acid magnalium inorganic gel is a raw material with magnesium hectorite mineral, follows these steps to be prepared:
1, the ore reduction of magnesium hectorite being become fineness with abrasive dust is 150-200 purpose breeze;
2, breeze is added water, stir into the ore pulp that weight percent concentration is 20-30%, add the viscosity-depression agent Sodium hexametaphosphate 99 in the time of stirring, the Sodium hexametaphosphate 99 consumption is the 0.2-0.5% of ore pulp solid content, and churning time is 50 minutes;
3, the gained ore pulp separates purification through two placed in-line hydrocyclones, removes impurity such as grit;
4, the ore pulp after the above-mentioned purification removes de-iron and oxide compound through 19600 Gausses' intensity magnetic separator;
5, the ore pulp after the above-mentioned purification enters modification for the first time, adds A type properties-correcting agent, i.e. Li
2SO
4And K
2SO
4, both ratios are 1: 5, and dosage is the 2-12% (dosage is 1-1.1 a times of cation exchange capacity in the ore pulp) of ore pulp solid content, and the control pH value is 5-5.5, and temperature of reaction is 80-90 ℃, the reaction times is 50 minutes;
6, after above-mentioned reaction finishes, carry out the modification second time: promptly add Type B properties-correcting agent MgSO
4With Al
2(SO
4)
3Mixture, the two weight ratio is 1: (1-1.5), dosage is the 1-1.5% of ore pulp solid content, control pH value be that 8-9 (uses Na
2CO
3Regulate pH value), temperature of reaction is 40-50 ℃, the reflection time is 10-20 minute.
7, the ore pulp that obtains by the reaction of the 6th step, concentrated through the horizontal screw unloading whizzer of continuous operating.
8, above-mentioned spissated ore pulp is washed with ethanol, mode of washing is vacuum filtration formula washing (for the washing of filter formula a kind of), the ethanol consumption be the ore pulp solid content 1.5-3.0 doubly, washing terminal point is not had Cl in the filtrate
-Detect, it is neutral that PH=7 is fully.Ethanol reclaims by the distiller distillation in the filtrate, and the ethanol of recovery injects ethanol storage tank, in order to using next time.
9, the ore pulp after above-mentioned washing with alcohol carries out air stream drying with pneumatic conveying dryer, is the powdered silicate magnalium inorganic gel product of 8-9% to obtain 60-150 purpose water content.The whiteness of product is 76%, and purity reaches 99.2%
With by above-mentioned 1-9 step process, resulting aluminium magnesium silicate inorganic gel powder-like product carries out glue: the colloid concentration according to 4%, 3000 rev/mins of rotating speeds, 30 minutes time, temperature is under 25 ℃ the condition, by homogenizer system gel colloid, record viscosity number 150-500mpa.s, thixotroping value 1.4-1.6, pH value 7 is better than the like product index that original technology obtains.
Claims (5)
1, a kind of preparation method of high purity silicic acid magnalium inorganic gel, comprise raw mineral materials is pulverized, breeze Jia Shui and with viscosity-depression agent slurrying, centrifugation is purified, add A type modifier modification, add the Type B modifier modification, ore pulp after twice modification is concentrated with whizzer, the colloidal ore pulp of handling is carried out aftertreatments such as drying, and its feature part is also to comprise the following steps:
(1) adopts the Wet-type strong magnetic separator deironing;
(2) adopt alcohol agent, the concentrated ore pulp after the purification modification is carried out the washing of filter formula.
2, preparation method according to claim 1 is characterized in that: in above-mentioned (1) step, the magneticstrength of described Wet-type strong magnetic separator is in 10000-25000 Gauss.
3, preparation method according to claim 2 is characterized in that: the preferable magneticstrength of described Wet-type strong magnetic separator is 18000-20000 Gauss.
4, preparation method according to claim 1 is characterized in that: in above-mentioned (2) step, described alcohol agent comprises methyl alcohol, ethanol, Virahol.
5, preparation method according to claim 4 is characterized in that: the 1.5-3.0 that described alcohol agent consumption is the ore pulp solid content doubly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410039840 CN1257103C (en) | 2004-03-22 | 2004-03-22 | Method for preparing inorganic gel of aluminium magnesium silicate in high purity |
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|---|---|---|---|
| CN 200410039840 CN1257103C (en) | 2004-03-22 | 2004-03-22 | Method for preparing inorganic gel of aluminium magnesium silicate in high purity |
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|---|---|
| CN1562745A true CN1562745A (en) | 2005-01-12 |
| CN1257103C CN1257103C (en) | 2006-05-24 |
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|---|---|---|---|
| CN 200410039840 Expired - Fee Related CN1257103C (en) | 2004-03-22 | 2004-03-22 | Method for preparing inorganic gel of aluminium magnesium silicate in high purity |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100388990C (en) * | 2006-08-25 | 2008-05-21 | 蒋文兰 | Production method of alcohol-based concave-convex stick suspending agent |
| CN100388991C (en) * | 2006-08-25 | 2008-05-21 | 蒋文兰 | Production method of water-based concave-convex stick suspending agent |
| CN102367856A (en) * | 2011-09-02 | 2012-03-07 | 芜湖禾田汽车工业有限公司 | Corrosion-resistant anti-freezing damping fluid for hydraulic suspension product of automotive engine |
| CN102374253A (en) * | 2011-09-02 | 2012-03-14 | 芜湖禾田汽车工业有限公司 | Damping fluid of hydraulic suspension product of automobile engine |
| CN103691371A (en) * | 2013-11-29 | 2014-04-02 | 苏州中材非金属矿工业设计研究院有限公司 | Electrolyte-resistant composite mineral gel |
| CN105600798A (en) * | 2015-12-29 | 2016-05-25 | 苏州中材非金属矿工业设计研究院有限公司 | Aluminium-magnesium silicate inorganic gel with good dispersity and preparing method thereof |
| CN106145129A (en) * | 2015-03-31 | 2016-11-23 | 神华集团有限责任公司 | A kind of coal ash for manufacturing is for the method for aluminium-magnesium silicate |
| CN107555445A (en) * | 2017-10-12 | 2018-01-09 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of aluminium magnesium silicate inorganic gel and preparation method thereof |
| CN115041107A (en) * | 2022-06-01 | 2022-09-13 | 芜湖硕华新材料科技有限公司 | Preparation method of temperature-resistant salt-tolerant high-performance inorganic gel |
-
2004
- 2004-03-22 CN CN 200410039840 patent/CN1257103C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100388990C (en) * | 2006-08-25 | 2008-05-21 | 蒋文兰 | Production method of alcohol-based concave-convex stick suspending agent |
| CN100388991C (en) * | 2006-08-25 | 2008-05-21 | 蒋文兰 | Production method of water-based concave-convex stick suspending agent |
| CN102367856A (en) * | 2011-09-02 | 2012-03-07 | 芜湖禾田汽车工业有限公司 | Corrosion-resistant anti-freezing damping fluid for hydraulic suspension product of automotive engine |
| CN102374253A (en) * | 2011-09-02 | 2012-03-14 | 芜湖禾田汽车工业有限公司 | Damping fluid of hydraulic suspension product of automobile engine |
| CN103691371A (en) * | 2013-11-29 | 2014-04-02 | 苏州中材非金属矿工业设计研究院有限公司 | Electrolyte-resistant composite mineral gel |
| CN103691371B (en) * | 2013-11-29 | 2016-03-16 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of Electrolyte-resistancomposite composite mineral gel |
| CN106145129A (en) * | 2015-03-31 | 2016-11-23 | 神华集团有限责任公司 | A kind of coal ash for manufacturing is for the method for aluminium-magnesium silicate |
| CN105600798A (en) * | 2015-12-29 | 2016-05-25 | 苏州中材非金属矿工业设计研究院有限公司 | Aluminium-magnesium silicate inorganic gel with good dispersity and preparing method thereof |
| CN107555445A (en) * | 2017-10-12 | 2018-01-09 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of aluminium magnesium silicate inorganic gel and preparation method thereof |
| CN115041107A (en) * | 2022-06-01 | 2022-09-13 | 芜湖硕华新材料科技有限公司 | Preparation method of temperature-resistant salt-tolerant high-performance inorganic gel |
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|---|---|
| CN1257103C (en) | 2006-05-24 |
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