Background technology
Metasilicate pentahydrate sodium is xln, and Relative bulk density is 0.8-1.0g/ml, fusing point 72.2 DEG C, and relative molecular weight is 212; Soluble in water and sig water, is insoluble to alcohol and acid, and the aqueous solution is in alkalescence, and dew puts easy moisture absorption deliquescence in air; Soil removability is strong, and PH surge capability is large; There is the performances such as good de-sludging emulsification, dispersion, moistening, infiltration.
Product, as washing auxiliary detergent, can substitute tripoly phosphate sodium STPP (STPP) and produce without phosphorus, low-phosphorous washing composition; As the main raw material of auxiliary agent, be widely used for fields such as the decontamination bleaching of the boiling and bleaching of cotton spinning etc., paper industry, paper deinking agent, ceramic grinding aid water reducer, cement water reducing agents in the pre-treatment of textile and dyeing industry; Meanwhile, be also widely used in chemical flame retardant for textile, flame-proofing agent raw material, protect and mould water-holding agent raw material, mineral oil recovery, the building aspect such as metallurgical industry dispersion agent and quick dry agent, oil drilling quick-setting additive, water conditioning.
Conventional production methods is be statically placed in by inclined silicon liquid in crystallizing pan and add a certain amount of crystal seed, crystallization is integrated at physical environment borehole cooling and in crystallizing pan, through artificial pneumatic pick, the metasilicate pentahydrate sodium of crystallization in crystallizing pan is broken into bulk, then obtains metasilicate pentahydrate sodium product after bulk material being put into pulverizer pulverizing.
The production technique of existing metasilicate pentahydrate sodium mainly has the following disadvantages: one is batch production method, and production efficiency is low, and operative's intensity is large; The natural cooling crystallization time is long, and summer, crystallization time reached more than 20 hours; Two is that after pulverizing, product purity is low, and without screening, its product grading is uneven, and particle surface is irregular, thus causes product whiteness low, the problems such as the storage time is short.
Summary of the invention
Technical problem to be solved by this invention is: the deficiency existed for prior art, provide a kind of crystallisation by cooling time short, production efficiency is high, and product purity is high, and can reduce the production method of the metasilicate pentahydrate sodium of producers' labour intensity.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A production method for metasilicate pentahydrate sodium, described production method comprises the following steps:
(1) with dioxide-containing silica be 99.3 ~ 100% quartz sand and sodium oxide content be that the caustic soda of 45 ~ 50% is for reaction raw materials, the weight ratio 1:1.5-1.8 of described quartz sand and described caustic soda, under the condition of pressure 0.6-1.6MPa, temperature 150-200 DEG C, react 4-12 hour, obtain the thick liquid of liquid sodium silicate;
(2) at 80-95 DEG C of temperature, in the thick liquid of liquid sodium silicate, add flocculation agent, stir 30-60 minute, leave standstill 10-15 hour, obtain flocculation liquid, in described flocculation liquid, add flocculating aids, device filters after filtration, obtains water glass refined liquid and filter residue;
(3) caustic soda being 50% by described water glass refined liquid and sodium oxide content mixes according to the ratio of weight ratio 1.5-2.5:1, and obtained silicon-dioxide and sodium oxide total content are the metasilicate pentahydrate sodium melt liquid of 55-60%;
(4) described metasilicate pentahydrate sodium melt liquid is cooled, in described metasilicate pentahydrate sodium melt liquid, pass into pressurized air while cooling, carry out airflow stirring, make the temperature of described metasilicate pentahydrate sodium melt liquid be cooled to 65-70 DEG C;
(5) above-mentioned cooled metasilicate pentahydrate sodium melt liquid and small-particle crystal seed are carried out abundant mix and blend, described metasilicate pentahydrate sodium melt liquid is made to be attached to described small-particle seed surface equably, again after cooling, make described metasilicate pentahydrate sodium melt liquid in described small-particle seed surface solidification crystallization;
(6) after crystallization, then through air-cooled or water-cooled, be cooled to less than 50 DEG C, sieve through 18-30 mesh sieve, to obtain final product.
Improve as one, in step (2), during filtration, when the inside and outside differential pressure of filtration unit is greater than 0.2MPa, increase the pressure at filtrate outlet place, when keeping filtering, the inside and outside differential pressure of described filtration unit is less than 0.2MPa, terminates until filter.
Improve as one, in step (2), the add-on of described flocculation agent is the 0.2-0.5 ‰ of the thick liquid weight of described liquid sodium silicate.
Improve as one, in step (2), described flocculation agent is polyacrylamide flocculation agent.
Improve as one, in step (2), the weight of described flocculating aids is the 0.2-2% of described flocculation liquid weight.
Improve as one, in step (2), described flocculating aids is the mixture of diatomite and gac, and the weight ratio of described diatomite and gac is 2:1.
Improve as one, in step (4), passing into described compressed-air actuated tolerance is 1-3m
3/ min, cooling time is 2-3 hour.
Improve as one, in step (5), the weight ratio of described small-particle crystal seed and described metasilicate pentahydrate sodium melt liquid is 1.5-3.5:1.
Improve as one, in step (5), Tc is 55-70 DEG C, and crystallization time is 5-20 minute.
Improve as one, in step (6), the macrobead after screening after crushed, crosses 40-60 mesh sieve, for subsequent use as crystal seed together with the fine powder after screening.
Owing to have employed technique scheme, the invention has the beneficial effects as follows:
Production method provided by the invention is continuous prodution, reaction, refining, filtration, melting, cooling, granulation and sieve each step and carry out in order; Wherein, during the refining filtering of the thick liquid of liquid sodium silicate, the use of flocculation agent makes the insoluble silicates such as iron in liquid, aluminium, calcium, magnesium flocculate into macromolecular particle by small molecules, after leaching, reduce foreign matter content, improve the purity of the finished product, the use in-depth of flocculating aids and the cake layer that loosened, reduce filtration resistance, improve filtering rate, and absorbed portion pigment and small molecular weight impurity, effectively extend filtration cycle, improve and stable filtering accuracy; Pass into pressurized air while melt liquid cooling, substantially reduce cooling time, make cooling evenly, reduce the viscosity of the rear liquid of cooling; Be cooled to less than 50 DEG C after crystallization, the temperature 55-70 DEG C of crystallization after its seeding temperature mixes with fluid temperature, can be reached; In whole production process, producers do not participate in the manufacture of product, only participate in the control and regulation of processing parameter, greatly reduce the labour intensity of producers.
Production method provided by the invention, the product obtained by this production method has higher purity and whiteness and product particle is even, surface is mellow and full, the index of the product obtained by the method is as follows: dioxide-containing silica: 27.8-29.2%, sodium oxide content: 28.7-30%, whiteness: > 85%, iron level: < 0.005%, granularity 18-30 order %:99%, water-insoluble: < 0.01%; This production method can realize continuous prodution, operational safety, reduces investment and running cost.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment one
A production method for metasilicate pentahydrate sodium, described production method comprises the following steps:
(1) get quartz sand (dioxide-containing silica is 99.3%) 25kg, caustic soda (sodium oxide content is 45%) 45kg, react 4 hours under the condition of pressure 1.6MPa, temperature 200 DEG C, obtain the thick liquid of liquid sodium silicate;
(2) at 80 DEG C, flocculation agent is added in the thick liquid of liquid sodium silicate, flocculation agent is preferably polyacrylamide flocculation agent, the add-on of flocculation agent is 0.2 ‰ of the thick liquid weight of liquid sodium silicate, stir 30 minutes, leave standstill 15 hours, must be flocculated liquid, flocculating aids is added in flocculation liquid, the weight of flocculating aids is 0.2% of flocculation liquid weight, and flocculating aids is the mixture of diatomite and gac, and the weight ratio of diatomite and gac is 2:1, device filters after filtration, obtains water glass refined liquid and filter residue;
(3) water glass refined liquid and caustic soda (sodium oxide content is 50%) are mixed according to the ratio of 1.5:1, obtained silicon-dioxide and sodium oxide total content are the metasilicate pentahydrate sodium melt liquid of 55-60%;
(4) metasilicate pentahydrate sodium melt liquid is cooled, in metasilicate pentahydrate sodium melt liquid, pressurized air is passed into while cooling, carry out airflow stirring, make the temperature of metasilicate pentahydrate sodium melt liquid be cooled to 65 DEG C, passing into compressed-air actuated tolerance is 1-3m
3/ min, cooling time is 2 hours;
(5) above-mentioned cooled metasilicate pentahydrate sodium melt liquid and small-particle crystal seed are carried out abundant mix and blend, the weight ratio of small-particle crystal seed and metasilicate pentahydrate sodium melt liquid is 1.5:1, metasilicate pentahydrate sodium melt liquid is made to be attached to small-particle seed surface equably, again after cooling, make metasilicate pentahydrate sodium melt liquid in small-particle seed surface solidification crystallization, Tc is 55 DEG C, and crystallization time is 20 minutes;
(6) after crystallization, then through air-cooled or indirect water-cooling, be cooled to less than 50 DEG C, sieve through 18-30 mesh sieve, to obtain final product.
Embodiment two
A production method for metasilicate pentahydrate sodium, described production method comprises the following steps:
(1) get quartz sand (dioxide-containing silica is 99.5%) 28kg, caustic soda (sodium oxide content is 48%) 42kg, react 8 hours under the condition of pressure 1.0MPa, temperature 180 DEG C, obtain the thick liquid of liquid sodium silicate;
(2) at 90 DEG C, flocculation agent is added in the thick liquid of liquid sodium silicate, flocculation agent is preferably polyacrylamide flocculation agent, the add-on of flocculation agent is 0.3 ‰ of the thick liquid weight of liquid sodium silicate, stir 45 minutes, leave standstill 13 hours, must be flocculated liquid, flocculating aids is added in flocculation liquid, the weight of flocculating aids is 1% of flocculation liquid weight, and flocculating aids is the mixture of diatomite and gac, and the weight ratio of diatomite and gac is 2:1, device filters after filtration, obtains water glass refined liquid and filter residue;
(3) water glass refined liquid and caustic soda (sodium oxide content is 50%) are mixed according to the ratio of 2:1, obtained silicon-dioxide and sodium oxide total content are the metasilicate pentahydrate sodium melt liquid of 55-60%;
(4) metasilicate pentahydrate sodium melt liquid is cooled, in metasilicate pentahydrate sodium melt liquid, pressurized air is passed into while cooling, carry out airflow stirring, make the temperature of metasilicate pentahydrate sodium melt liquid be cooled to 70 DEG C, passing into compressed-air actuated tolerance is 1-3m
3/ min, cooling time is 3 hours;
(5) above-mentioned cooled metasilicate pentahydrate sodium melt liquid and small-particle crystal seed are carried out abundant mix and blend, the weight ratio of small-particle crystal seed and metasilicate pentahydrate sodium melt liquid is 2.5:1, metasilicate pentahydrate sodium melt liquid is made to be attached to small-particle seed surface equably, again after cooling, make metasilicate pentahydrate sodium melt liquid in small-particle seed surface solidification crystallization, Tc is 63 DEG C, and crystallization time is 13 minutes;
(6) after crystallization, then through air-cooled or indirect water-cooling, be cooled to less than 50 DEG C, sieve through 18-30 mesh sieve, to obtain final product.
Embodiment three
A production method for metasilicate pentahydrate sodium, described production method comprises the following steps:
(1) get quartz sand (dioxide-containing silica is 100%) 30kg, caustic soda (sodium oxide content is 50%) 48kg, react 12 hours under the condition of pressure 0.6MPa, temperature 150 DEG C, obtain the thick liquid of liquid sodium silicate;
(2) at 95 DEG C, flocculation agent is added in the thick liquid of liquid sodium silicate, flocculation agent is preferably polyacrylamide flocculation agent, the add-on of flocculation agent is 0.5 ‰ of the thick liquid weight of liquid sodium silicate, stir 60 minutes, leave standstill 10 hours, must be flocculated liquid, flocculating aids is added in flocculation liquid, the weight of flocculating aids is 2% of flocculation liquid weight, and flocculating aids is the mixture of diatomite and gac, and the weight ratio of diatomite and gac is 2:1, device filters after filtration, obtains water glass refined liquid and filter residue;
(3) water glass refined liquid and caustic soda (sodium oxide content is 50%) are mixed according to the ratio of 2.5:1, obtained silicon-dioxide and sodium oxide total content are the metasilicate pentahydrate sodium melt liquid of 55-60%;
(4) metasilicate pentahydrate sodium melt liquid is cooled, in metasilicate pentahydrate sodium melt liquid, pressurized air is passed into while cooling, carry out airflow stirring, make the temperature of metasilicate pentahydrate sodium melt liquid be cooled to 70 DEG C, passing into compressed-air actuated tolerance is 1-3m
3/ min, cooling time is 3 hours;
(5) above-mentioned cooled metasilicate pentahydrate sodium melt liquid and small-particle crystal seed are carried out abundant mix and blend, the weight ratio of small-particle crystal seed and metasilicate pentahydrate sodium melt liquid is 3.5:1, metasilicate pentahydrate sodium melt liquid is made to be attached to small-particle seed surface equably, again after cooling, make metasilicate pentahydrate sodium melt liquid in small-particle seed surface solidification crystallization, Tc is 70 DEG C, and crystallization time is 5 minutes;
(6) after crystallization, then through air-cooled or indirect water-cooling, be cooled to less than 50 DEG C, sieve through 18-30 mesh sieve, to obtain final product.
Embodiment four
A production method for metasilicate pentahydrate sodium, described production method comprises the following steps:
(1) get quartz sand (dioxide-containing silica is 99.5%) 26kg, caustic soda (sodium oxide content is 50%) 44.2kg, react 6 hours under the condition of pressure 1.6MPa, temperature 200 DEG C, obtain the thick liquid of liquid sodium silicate;
(2) at 95 DEG C, flocculation agent is added in the thick liquid of liquid sodium silicate, flocculation agent is preferably polyacrylamide flocculation agent, the add-on of flocculation agent is 0.5 ‰ of the thick liquid weight of liquid sodium silicate, stir 60 minutes, leave standstill 10 hours, must be flocculated liquid, flocculating aids is added in flocculation liquid, the weight of flocculating aids is 2% of flocculation liquid weight, flocculating aids is the mixture of diatomite and gac, the weight ratio of diatomite and gac is 2:1, device filters after filtration, during filtration, when the inside and outside differential pressure of filtration unit is greater than 0.2MPa, increase the pressure at filtrate outlet place, when keeping filtering, the inside and outside differential pressure of filtration unit is less than 0.2MPa, terminate until filter, obtain water glass refined liquid and filter residue,
(3) water glass refined liquid and caustic soda (sodium oxide content is 50%) are mixed according to the ratio of 2.5:1, obtained silicon-dioxide and sodium oxide total content are the metasilicate pentahydrate sodium melt liquid of 55-60%;
(4) metasilicate pentahydrate sodium melt liquid is cooled, in metasilicate pentahydrate sodium melt liquid, pressurized air is passed into while cooling, carry out airflow stirring, make the temperature of metasilicate pentahydrate sodium melt liquid be cooled to 70 DEG C, passing into compressed-air actuated tolerance is 1-3m
3/ min, cooling time is 3 hours;
(5) above-mentioned cooled metasilicate pentahydrate sodium melt liquid and small-particle crystal seed are carried out abundant mix and blend, the weight ratio of small-particle crystal seed and metasilicate pentahydrate sodium melt liquid is 3.5:1, metasilicate pentahydrate sodium melt liquid is made to be attached to small-particle seed surface equably, again after cooling, make metasilicate pentahydrate sodium melt liquid in small-particle seed surface solidification crystallization, Tc is 70 DEG C, and crystallization time is 5 minutes;
(6) after crystallization, then through air-cooled or indirect water-cooling, be cooled to less than 50 DEG C, sieve through 18-30 mesh sieve, obtain described product, the macrobead after screening after crushed, crosses 40-60 mesh sieve, for subsequent use as crystal seed together with the fine powder after screening.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.