CN102303888B - Production method of caking-proof strontium chloride hexahydrate - Google Patents
Production method of caking-proof strontium chloride hexahydrate Download PDFInfo
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- CN102303888B CN102303888B CN 201110228787 CN201110228787A CN102303888B CN 102303888 B CN102303888 B CN 102303888B CN 201110228787 CN201110228787 CN 201110228787 CN 201110228787 A CN201110228787 A CN 201110228787A CN 102303888 B CN102303888 B CN 102303888B
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Abstract
The invention relates to a production method of strontium chloride hexahydrate for liquid crystal glass base plate production. The production method comprises the following steps: a, concentrating a strontium chloride solution at the temperature of less than 100 DEG C to 38-44 baume degrees; b, cooling and crystallizing the solution, wherein the specifically steps are as follows: firstly adding crystal seeds, which are strontium chloride hexahydrate crystals with a particle diameter of less than 1 millimeter, at the charging ratio above 2 kg/m<3> and controlling cooling speed; c, ageing a crystal slurry solution reaching the temperature for 1.5-3 hours under the stirring condition; and d, putting aged crystal slurry in an automatic centrifugal machine for dehydration, and drying with cold wind so as to obtain a finished product. According to the production method provided by the invention, the surface of the strontium chloride hexahydrate crystal has extremely low adhered water and low impurities; by a stacking test for 6 months, no caking phenomenon occurs; and by a stacking test for 9 months, little caking phenomenon occurs (the ratio of caking is 5-8%), and the cakes can be loosened by lightly pinching with hands.
Description
Technical field
The present invention relates to the production method of six water strontium chlorides, especially be mainly used in the six water strontium chlorides that the production of liquid crystal glass base is used.
Background technology
Due to liquid crystal glass base to the raw material mixture homogeneity require highly, require all formula materials to have fabulous shatter value so that the mixing of raw material, reduce the scrap rate of its product.
And six water strontium chlorides are one of most important raw materials in liquid crystal glass base production, the production technique of present six water strontium chlorides is mainly: by add the organism that contains the hydrophobic group in six water strontium chloride products, be coated on the surface of six water strontium chloride crystal, in prior art, similarly the anti-hard caking agent kind is also many, and such method can play certain preventing blocking effect.
But there are following two serious defectives: 1, all contain the objectionable constituent such as phenyl group due to the additive that adds, in production process with in using, all environment is brought pollution, HUMAN HEALTH is had disadvantageous effect; 2, anti-caking is generally 2-3 month working lipe, and in the situation of product long-distance transport or standing storage, anti-hard caking agent lost efficacy, and product still can lump, and is unfavorable for the production and application of liquid crystal glass base; 3, the anti-hard caking agent that joins in six water strontium chloride products can enter in the Liquid crystal production system, but for liquid crystal glass base, anti-hard caking agent etc. are organic is but impurity, and the introducing of these impurity brings bad impact must for the quality of liquid-crystalline glasses substrate.
Summary of the invention
Purpose of the present invention will provide a kind of to be had good agglomeration preventing performance and not to contain again anti-caking additive, and liquid crystal glass base is produced the production method of six special-purpose water strontium chlorides.
Technical scheme of the present invention is: a kind of production method of anti-caking six water strontium chlorides, and step comprises:
A, strontium chloride solution is concentrated to 38～44 degree Beaume at lower than the temperature of 100 ℃;
B, solution is carried out crystallisation by cooling, concrete steps are: at first add crystal seed, crystal seed is particle diameter less than the six water strontium chloride crystal of 1 millimeter, and feed ratio is 2kg/m
3Above; Cooling rate is: solution temperature is before 48 ℃, and the cooling medium is natural wind, and cooling rate is 2 ℃/hour; Solution temperature is when 40～48 ℃ of scopes, and the cooling medium is the normal-temperature water of 25 ℃, and cooling rate is 1.2 ℃/hour; Solution temperature is less than 40 ℃, and the cooling medium is that temperature is the refrigerated water of 8 ℃, and cooling rate is 1.5 ℃/hour, solution is cooled to 15 ℃ always;
C, will reach the ageing 1.5～3 hours under agitation condition of magma solution after temperature;
D, the magma that ageing is good are put into the automatic centrifuge dehydration, then get finished product with cold air drying.
The rotating speed of stirring wherein is definite according to the size of agitator, and size is larger, and linear velocity is larger, and stirring velocity just can be suitably slow so, otherwise just hurry up.But follow first slow after fast principle, be as for concrete data that those skilled in the art need not creative work according to practical situation namely confirmable, as long as can play the effect of homogenizing material, itself neither improvement of the present invention.And stirring velocity can be controlled by automatic control system, has arrived the specified temperature scope namely automatically by adjusting step-down gear current reduction stir speed (S.S.) as solution temperature.
The contriver passes through long-term observation and thinks: the major cause of strontium chloride caking is as follows: (1) six water strontium chloride crystal water dehydration temperature is lower, wherein two crystal water just begin to lose at 54 ℃, thereby cause the crystal recrystallization and lump, more easily producing this phenomenon when especially heating up because of factors such as Exposures to Sunlight in the transportation of product with in storing.(2) there is attached water in plane of crystal, because the variation of crystalline temp and pressure causes the crystal recrystallization, thereby causes caking.(3) under usual condition, when six water strontium chloride crystal do not carry out crystallization control, easily generate tiny needle-like crystal, specific surface area is large, easily play the bridging effect between crystal and crystal, slightly being under pressure local dissolution more easily occurs with temperature variation, and recrystallization causes caking.
In technical scheme of the present invention: mainly take following several respects measure to improve the agglomeration problems of six water strontium chlorides: (1) changes the physicals of crystal own, namely by the crystallization control process, making crystal shape is to be converted into particulate state by needle-like, and crystallographic dimension is changed into particle diameter roughly at the particle of 1～8 mm in size by the needle-like crystal of common 0.2* (1～2) millimeter; (2) product is carried out cold wind and dry up, thoroughly remove the attached water of plane of crystal; Prevent the recrystallization of crystal.Require to want the namely cooling crystal water of condensation in absorbed air again after the warm air drying of cold air drying herein.In other words technological core of the present invention also can be regarded as by changing the crystallisation process of strontium chloride, has changed the crystalline structure of six water strontium chlorides, has become the particulate state crystal by needle-like crystal, and the size of crystal is controlled by mixing speed.Although particle dress crystal is very common in Chemicals, but granular six water strontium chloride crystal also are not made, and such particle diameter has outstanding advantage at the particulate state six water strontium chloride crystal of 1～3 millimeter aspect agglomeration resistance, can guarantee 6～7 months without caking phenomenon in the situation that do not need to add any anti-caking additive.Not only have than the use better anti-caking effect of additive but also reduced cost, and being beneficial to the quality raising of liquid crystal glass base.Namely the present invention changes crystallization and controls index, and the particulate state six water strontium chloride crystal that make have unexpected effect aspect anti-caking effect.
Specifically: six such water strontium chloride planes of crystal adhere to that water electrode is low and foreign matter content is low.Process reaches the stacking test of 6 months, without caking phenomenon, through the stacking test of 9 months, a small amount of caking phenomenon (the caking ratio is 5～8%) is arranged, but pinch just loose with have gentle hands.
Further improve and be: in described step b, the crystal seed add-on is controlled at 5kg/m
3Usually crystal seed is more, and the particle diameter of the crystal of gained is larger, but the strontium chloride content in solution is limited, so particle diameter neither be infinitely-great, considers source and the Cost Problems of crystal seed, and the crystal seed add-on is at 20kg/m
3In, particle diameter is accordingly at 1～8 millimeter.What the crystal seed add-on was best is at 2～5kg/m
3, coordinating suitable mixing speed, crystal particle diameter concentrates on 2～3 millimeters, and ultimate value is at 1～4 millimeter.Such particle diameter is the most reasonable, has best agglomeration preventing performance through experiment confirm.
Further, in described steps d, the crystal after centrifugal utilizes vibrated fluidized bed to carry out cold wind and dries up; Utilize simultaneously cold wind that major part is blown to tornado dust collector less than the fine crystals of 1 millimeter particle diameter and reclaim, use as crystal seed.
Further, in described step a, strontium chloride solution is concentrated to 40 degree Beaume.Crystallization effect is best like this, and when this concentration, crystal is mobility under agitation, avoids the crystal collision to cause that crystal modification is even broken.Certainly can not be too rare, increase the energy consumption of crystallisation by cooling.
In described step b, c, stirring velocity speed when temperature is higher is fast, and when temperature is low, speed is slow.
In described step c, digestion time is 2 hours.Can guarantee so thoroughly make the strontium chloride crystallization and grow up gradually, efficiency is saved most simultaneously.
Embodiment
For making those skilled in the art's more detailed understanding using method of the present invention and technique effect, provide following examples and the corresponding data that detect.
Embodiment one
Strontium chloride solution is concentrated to 38 degree Beaume under 95 ℃,
The crystal seed feed ratio is 2kg/m
3Method of cooling is carried out according to requirement of the present invention;
The ageing 1.5 hours under agitation condition of magma solution;
The dehydration of magma automatic centrifugation, then dry in the air and get finished product 1 with cold air drying in the beach.
Embodiment two
Strontium chloride solution is concentrated to 40 degree Beaume under 90 ℃,
The crystal seed feed ratio is 3kg/m
3Method of cooling is carried out according to requirement of the present invention;
The ageing 2 hours under agitation condition of magma solution;
Magma automatic centrifugation dehydration, the crystal after centrifugal utilize vibrated fluidized bed to carry out cold wind and dry up and obtain finished product 2; Utilize simultaneously cold wind that major part is blown to tornado dust collector less than the fine crystals of 1 millimeter particle diameter and reclaim, use as crystal seed.
Embodiment three
Strontium chloride solution is concentrated to 40 degree Beaume under 95 ℃,
The crystal seed feed ratio is 4kg/m
3Method of cooling is carried out according to requirement of the present invention;
The ageing 2.5 hours under agitation condition of magma solution;
Magma automatic centrifugation dehydration, the crystal after centrifugal utilize vibrated fluidized bed to carry out cold wind and dry up and obtain finished product 3; Utilize simultaneously cold wind that major part is blown to tornado dust collector less than the fine crystals of 1 millimeter particle diameter and reclaim, use as crystal seed.
Embodiment four
Strontium chloride solution is concentrated to 40 degree Beaume under 100 ℃,
The crystal seed feed ratio is 5kg/m
3Method of cooling is carried out according to requirement of the present invention;
The ageing 2 hours under agitation condition of magma solution;
Magma automatic centrifugation dehydration, the crystal after centrifugal utilize vibrated fluidized bed to carry out cold wind and dry up and obtain finished product 4; Utilize simultaneously cold wind that major part is blown to tornado dust collector less than the fine crystals of 1 millimeter particle diameter and reclaim, use as crystal seed.
Embodiment five
Strontium chloride solution is concentrated to 44 degree Beaume under 95 ℃,
The crystal seed feed ratio is 5kg/m
3Method of cooling is carried out according to requirement of the present invention;
The ageing 3 hours under agitation condition of magma solution;
Magma automatic centrifugation dehydration, the crystal after centrifugal utilize vibrated fluidized bed to carry out cold wind and dry up and obtain finished product 5; Utilize simultaneously cold wind that major part is blown to tornado dust collector less than the fine crystals of 1 millimeter particle diameter and reclaim, use as crystal seed.
Embodiment six
Strontium chloride solution is concentrated to 42 degree Beaume under 95 ℃,
The crystal seed feed ratio is 4kg/m
3Method of cooling is carried out according to requirement of the present invention;
The ageing 2 hours under agitation condition of magma solution;
Magma automatic centrifugation dehydration, the crystal after centrifugal utilize vibrated fluidized bed to carry out cold wind and dry up and obtain finished product 6; Utilize simultaneously cold wind that major part is blown to tornado dust collector less than the fine crystals of 1 millimeter particle diameter and reclaim, use as crystal seed.
Six groups of above-mentioned samples carry out stacking test, and take the standard that caking rate ends as detection more than 5%, test is recorded a demerit as shown in table 1:
Table one: the result of product stacking test
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | |
| 6 months | Nothing | Nothing | Nothing | Nothing | Nothing | Nothing |
| 7 months | Nothing | Nothing | Nothing | Nothing | Nothing | Have |
| 8 months | Have | Nothing | Nothing | Nothing | Nothing | / |
| 9 months | / | Nothing | Nothing | Nothing | Nothing | / |
| 10 months | / | Have | Nothing | Nothing | Nothing | / |
| 11 months | / | / | Nothing | Have | Have | / |
| 12 months | / | / | Have | / | / | / |
| Median size | 2.2mm | 2.8mm | 2.7mm | 3.0mm | 2.9mm | 3.1mm |
By the above results as seen, the six water strontium chloride crystal that method of the present invention is produced guarantee 6 months at least without caking, extend than prior art and do not lump the phase more than one times, what have can reach 11 months, and month all comparatively loose with interior caking in half a year to 9, be easy to be fit to the production and application of liquid crystal glass base by the external force fragmentation.
Claims (6)
1. the production method of anti-caking six water strontium chlorides, step comprises:
A, strontium chloride solution is concentrated to 38～44 degree Beaume at lower than the temperature of 100 ℃;
B, solution is carried out crystallisation by cooling, concrete steps are: at first add crystal seed, crystal seed is particle diameter less than the six water strontium chloride crystal of 1 millimeter, and feed ratio is 2kg/m
3Above; Cooling rate is: solution temperature is before 48 ℃, and the cooling medium is natural wind, and cooling rate is 2 ℃/hour; Solution temperature is when 40～48 ℃ of scopes, and the cooling medium is the normal-temperature water of 25 ℃, and cooling rate is 1.2 ℃/hour; Solution temperature is less than 40 ℃, and the cooling medium is that temperature is the refrigerated water of 8 ℃, and cooling rate is 1.5./ hour, solution is cooled to 15 ℃ always;
C, will reach the ageing 1.5～3 hours under agitation condition of magma solution after temperature;
D, the magma that ageing is good are put into the automatic centrifuge dehydration, then get finished product with cold air drying.
2. production method according to claim 1, it is characterized in that: in described step b, the crystal seed add-on is controlled at 5kg/m
3
3. production method according to claim 1 is characterized in that: in described steps d, the crystal after centrifugal utilizes vibrated fluidized bed to carry out cold wind and dries up; Utilize simultaneously cold wind that major part is blown to tornado dust collector less than the fine crystals of 1 millimeter particle diameter and reclaim, use as crystal seed.
4. production method according to claim 1, it is characterized in that: in described step a, strontium chloride solution is concentrated to 40 degree Beaume.
5. production method according to claim 1, it is characterized in that: in described step b, c, stirring velocity speed when temperature is higher is fast, and when temperature is low, speed is slow.
6. production method according to claim 1, it is characterized in that: in described step c, digestion time is 2 hours.
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| CN 201110228787 CN102303888B (en) | 2011-08-10 | 2011-08-10 | Production method of caking-proof strontium chloride hexahydrate |
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| CN 201110228787 CN102303888B (en) | 2011-08-10 | 2011-08-10 | Production method of caking-proof strontium chloride hexahydrate |
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| CN104211101B (en) * | 2014-09-03 | 2016-03-23 | 华东理工大学 | A kind of preparation method of coarse sand shape six water strontium chloride |
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| CN102092759B (en) * | 2009-12-09 | 2013-01-16 | 贵州红星发展股份有限公司 | Method for preparing strontium dichloride hexahydrate |
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Address after: 402365 cologong village 3, cologong Town, Dazu District, Chongqing Patentee after: CHONGQING YUANHE FINE CHEMICALS INC. Address before: 400020 cologong village three, Cologne village, Dazu County, Chongqing Patentee before: Chongqing Yuanhe Fine Chemicals Co., Ltd. |