CN113880099B - Method for preparing sodium silicate by recycling organic silicon three wastes in green manner - Google Patents
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Abstract
The invention relates to a method for preparing sodium silicate by using three wastes of organic silicon for green recycling, belonging to the technical field of organic silicon. The invention comprises the following steps: (1) Incinerating three wastes containing silicon to obtain solid-phase siliceous ash slag; (2) Mixing, heating and stirring the silicon-containing ash slag and the waste alkali liquid, and then centrifugally separating solid and liquid phases; (3) The liquid phase enters a stirring kettle, the waste acid liquid is added into the stirring kettle, the liquid phase is discharged, and the solid phase silicic acid is left in the stirring kettle; (4) Adding waste alkali liquid into a stirring kettle containing solid-phase silicic acid, adding toluene, heating with water for reflux, fine-tuning the modulus of sodium silicate solution, and separating and recovering. The invention has scientific and reasonable design, fully utilizes the three wastes containing silicon, waste lye and waste acid liquor, is green and environment-friendly, achieves the purpose of generating high-value products by mutual-gram waste, and has high industrial application value.
Description
Technical Field
The invention relates to a method for preparing sodium silicate by using three wastes of organic silicon for green recycling, belonging to the technical field of organic silicon.
Background
A great deal of three wastes, namely waste liquid, waste solid and waste gas, are generated in the production process from the synthesis of methyl chloride to the production of middle and downstream products in the production chain of organosilicon monomer enterprises. The main component of the three wastes contains silicon element or exists in the modes of silicon methyl bond, silicon-chlorine bond, silicon-oxygen-silicon bond and the like. The three wastes of the organic silicon are mostly classified into dangerous wastes, and the treatment cost of the dangerous wastes is very high, so that the dangerous wastes not only do not generate benefits, but also can cause raw material waste and occupy production cost, and the dangerous waste treatment cost is an important component of the production cost of a single enterprise.
The current process for preparing sodium silicate is various: high temperature calcination of fly ash and sodium carbonate, wet reaction of quartz and caustic soda, wet reaction of rice hull ash and caustic soda, and the like. From the process characteristics of these methods, their drawbacks are as follows:
the patent CN201911396101.4 adopts fly ash and sodium carbonate to prepare sodium silicate after high-temperature roasting, water-dissolving, decoloring and flocculating agent purifying. The disadvantages of this process are: high-temperature roasting is needed, and the energy consumption is high; the activated carbon is required to be decolorized, and the used activated carbon is treated, so that the treatment cost is obviously increased; the flocculant is needed, and the flocculant is recycled in the later period, so that the recycling is incomplete and the pollution to the environment is necessarily caused; from these points, the process disadvantage of recovering silicon element from fly ash is very obvious.
Patent CN105271276a adopts a wet process of quartz sand and caustic soda to prepare sodium silicate. And (3) dropwise adding ammonia water after the quartz reacts with caustic soda, and then heating and reacting the silica gel with the rest caustic soda solution to prepare sodium silicate. There are two problems with this process: the quartz sand contains a large amount of impurity elements such as heavy metals and the problem of color, and the patent does not clearly show how to eliminate heavy metal ions and decolorize, and the application of sodium silicate in other fields is limited without decolorization and impurity removal; the characteristic that ammonia water is easily dissolved in water is adopted for reaction, so that the odor of sodium silicate solution is necessarily caused, and therefore, the problem of excessive ammonia water is solved, and the patent is not explicitly stated.
Patent CN101456555a provides a method for recovering elemental silicon from rice hull ash, which is a wet process for recovering silica. The patent first further pulverizes the rice hull ash and then soaks it with 2mol/L (about 8%) NaOH solution and heats it to produce sodium silicate. The patent also has the problem that the sodium silicate solution is colored after the rice hull ash is soaked and needs to be decolorized. And the article "a new process for producing high modulus water glass and activated carbon by using rice husk ash as raw material" has previously disclosed a method for recovering silicon dioxide from rice husk ash: heating and pressure up to 6 kg are required to recover the silica at a high leaching rate (about 90%). The operation under pressure certainly increases the difficulty of the process production. Therefore, although the rice husk ash is a method for recovering silicon element, the method cannot be used for large-scale industrial recovery of three wastes of organic silicon monomer enterprises due to the problems of pressurized operation, decoloration and the like, and has limited application prospect.
Disclosure of Invention
The invention aims to solve the technical problems that: the method for preparing sodium silicate by recycling the organic silicon three wastes is scientific and reasonable in design, fully utilizes the three wastes containing silicon, waste alkali liquid and waste acid liquid, is environment-friendly, achieves the purpose of generating high-value products by waste mutual gram, and has high industrial application value.
The invention relates to a method for preparing sodium silicate by using three wastes of green recycled organic silicon, which comprises the following steps:
(1) Incinerating the three wastes containing silicon at 900-1300 ℃ for 1-5s to obtain solid-phase siliceous ash slag;
(2) Mixing the silicon-containing ash with waste alkali liquor, heating and stirring for 1-8h at 80-100 ℃, introducing into a centrifuge, and performing first centrifugal separation to obtain solid and liquid phases;
(3) The liquid phase enters a stirring kettle, waste acid liquid is added into the stirring kettle, stirring is carried out for 0.5-3h, sodium silicate is converted into solid-phase silicic acid, the liquid phase is discharged (metal ions and the like are left in the liquid phase without decolorization), and the solid-phase silicic acid is left in the stirring kettle;
(4) Adding waste alkali liquor into a stirring kettle containing solid-phase silicic acid, dissolving the silicic acid again, then adding toluene, heating with water at 110-130 ℃ for reflux, finely adjusting modulus to ensure fluidity of sodium silicate solution, separating liquid to recover upper toluene, and obtaining lower sodium silicate solution with a certain modulus.
In the three wastes containing silicon, waste gas is waste gas and exhaust gas generated at the upstream and downstream of an organosilicon monomer production enterprise, such as monomer synthesis exhaust gas, rectification exhaust gas, tank area exhaust gas, cracking disproportionation exhaust gas, chloromethane synthesis, cracking pressurizing exhaust gas, water cracking ring and downstream deep processing exhaust gas; the waste solids are hydrolysate of a tail gas water washing system of the monomer synthesis device, slurry residue hydrolysate and semisolid sticky matters of the chloromethane synthesis device; the waste liquid is slurry slag generated by synthesizing the organic silicon monomer, an organic silicon cracking kettle substrate, an azeotrope of the organic silicon monomer, an organic silicon disproportionation kettle substrate, methyl silicic acid generated by a comprehensive utilization device, water scrubber oily matters and alkaline residues.
In the three wastes containing silicon, the main components are monomers or monomer mixtures (gas phase and liquid phase) containing the silicon methyl and the silicon-chlorine bond, and organic silicon hydrolysates (liquid phase and solid phase) containing the silicon-oxygen bond. The main components of ash slag generated by high-temperature incineration of the components are SiO 2 The silicon-containing ash is SiO 2 The incineration residue with the mass content more than 98.5 percent has high recycling value.
The waste alkali liquid and the waste acid liquid are both generated in the production operation of the organic silicon chloromethane synthesis device.
The alkali content in the waste alkali liquor is 5-8wt%; the HCl content in the waste acid liquid is 20-27wt%.
The reversible conversion of the silicic acid and the sodium silicate in the steps (3) and (4) can be repeatedly carried out for 1 to 5 times, namely, adding waste acid to convert the sodium silicate into the silicic acid, then adding waste alkali liquor to convert the silicic acid into the sodium silicate, and finally converting the silicic acid into the silicic acid. The repeated aim is to continuously dissolve impurities, such as heavy metal ions, which are coated and mixed in the silicic acid and lead to the solution color, in the liquid phase, ensure the purity of the silicic acid, be favorable for finally obtaining colorless sodium silicate solution, and omit the step of decoloring the sodium silicate solution.
In the step (4), preferably, the water reflux time is 0.5-5h, and the lower sodium silicate solution has excellent fluidity and can be smoothly discharged out of the reaction kettle after stirring, standing and layering. The water-carrying reflux step is used for finely adjusting the water content of the sodium silicate solution, so as to adjust the content of silicon dioxide, namely the modulus, to prevent the mobility of the sodium silicate solution from being deteriorated due to the excessively high modulus, so that the product cannot be smoothly discharged out of the reaction kettle, and production accidents are caused.
In the reversible conversion of different forms of sodium silicate and silicic acid, the chemical reaction equation involved is as follows:
the invention fully considers the composition characteristics of three wastes in the production enterprises of the organic silicon monomers, and trace the source to recycle the silicon element existing in the three wastes of the organic silicon in a mode of easy conversion and recovery (namely silicon dioxide), thereby reducing the waste of the silicon element and the treatment cost of the three wastes. Specifically, the main components of three wastes are substances existing in gas-liquid-solid states, such as silicon-containing monomers, monomer mixtures, hydrolysates and the like. These wastes contain a large amount of silicon element and are too high in cost for post-treatment as hazardous wastes, resulting in extremely high production costs for monomer production enterprises. The invention changes the three wastes into ash slag containing more than 98.5 percent of silicon dioxide components after incineration, and has high recovery value. Meanwhile, the waste alkali liquor and the waste acid liquor generated by the organic silicon monomer methyl chloride synthesis process are fully utilized, the silicon element is recovered in a sodium silicate mode by utilizing the reversible characteristic of sodium silicate and silicic acid, the process is a green process for converting three wastes into high-quality products, the waste generated by organic silicon monomer enterprises is mutually utilized to finish the preparation of the sodium silicate, and a green and environment-friendly method is provided for recycling the waste of the organic silicon monomer enterprises.
The invention aims to recover silicon element by taking three wastes containing silicon of an organic silicon monomer enterprise as raw materials and waste acid and alkali of the organic silicon monomer enterprise as an auxiliary agent. The modulus of the prepared sodium silicate can be specifically adjusted according to the requirements of the later application field of the sodium silicate.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention takes green and environment-friendly as concept, fully utilizes the three wastes characteristic of organic silicon monomer enterprises, namely the main component contains silicon element, takes the waste alkali liquor and the waste acid liquor of the chloromethane synthesizing device of the organic silicon monomer enterprises as the auxiliary agent for recovering the silicon element, realizes the chemical reaction of the three wastes containing silicon and the waste alkali liquor and the waste acid liquor, achieves the purpose of generating high-value products by mutual g of waste, and has high industrial application value;
(2) The method skillfully utilizes reversible conversion (as shown by a chemical reaction equation) of different forms of sodium silicate and silicic acid to fully separate colored substances from the silicic acid, and can realize the decolorization treatment of the sodium silicate solution without adopting a conventional decolorizing agent, so that the decolorization operation is abandoned, and the decolorization cost is reduced;
(3) According to the invention, toluene is taken as a water-carrying agent, a part of water is taken as a sodium silicate solution, the formation of sodium silicate is promoted, the modulus of the sodium silicate is finely adjusted, the hidden danger that the fluidity of the sodium silicate is poor and the sodium silicate cannot be discharged out of production equipment due to the excessively high modulus is eliminated, and the toluene can be easily separated from the sodium silicate solution through layering, so that the full recycling is realized.
Detailed Description
The invention is further illustrated below with reference to examples.
Example 1
And (3) burning the three wastes containing silicon at 950+/-30 ℃ for 1s to obtain solid-phase siliceous dust slag. Mixing the silica-containing ash slag with 5% waste alkali liquor, stirring at 80 ℃ for 8 hours, and then introducing the mixture into a centrifuge for first centrifugal separation of solid and liquid phases; the liquid phase enters a stirring kettle, 20% of waste acid liquid is added into the stirring kettle and stirred for 3 hours, sodium silicate is converted into solid-phase silicic acid, the liquid phase is discharged, and the solid-phase silicic acid is left in the stirring kettle; adding 5% waste alkali liquor into a stirring kettle containing solid-phase silicic acid again, dissolving silicic acid again, adding toluene, heating and refluxing for carrying water for 0.5h at 110 ℃, layering sodium silicate solution and toluene, wherein the lower layer is sodium silicate solution with good fluidity (modulus is 3.2-3.9) and slight yellow, and the upper layer toluene is recycled.
Example 2
And (3) burning the three wastes containing silicon at 1000+/-50 ℃ for 3 seconds to obtain solid-phase siliceous dust slag. Mixing the silica-containing ash slag with 5% waste alkali liquor, heating at 90 ℃, stirring, and then introducing into a centrifuge for first centrifugal separation of solid and liquid phases; the liquid phase enters a stirring kettle, 24% of waste acid liquid is added into the stirring kettle to be stirred for 2 hours, sodium silicate is converted into solid-phase silicic acid, the liquid phase is discharged, and the solid-phase silicic acid is left in the stirring kettle; adding 5% of waste alkali liquor into a stirring kettle containing solid-phase silicic acid again to dissolve the silicic acid; then, repeating the process for 1 time by using 24 percent of waste acid and 5 percent of waste alkali liquor to convert sodium silicate into silicic acid and then into sodium silicate; then toluene is added into the sodium silicate solution, water is added into the solution for 5 hours after the solution is heated at 110 ℃, the sodium silicate solution and the toluene are layered, the lower layer is colorless and transparent sodium silicate solution with excellent fluidity (modulus is 1.2-2.2), and the upper layer toluene is recycled.
Example 3
And (3) burning the three wastes containing silicon for 4s at 1100+/-20 ℃ to obtain solid-phase siliceous dust slag. Mixing the siliceous dust slag with 6% waste alkali liquor, heating at 100 ℃, stirring, and then introducing into a centrifuge for first centrifugal separation of solid and liquid phases; the liquid phase enters a stirring kettle, 27% of waste acid liquid is added into the stirring kettle to be stirred for 1h, sodium silicate is converted into solid-phase silicic acid, the liquid phase is discharged, and the solid-phase silicic acid is left in the stirring kettle; adding 6% of waste alkali liquor into a stirring kettle containing solid-phase silicic acid again to dissolve the silicic acid, and then repeating the process for 2 times by using 27% of waste acid and 6% of waste alkali liquor to convert sodium silicate into silicic acid and then sodium silicate; then toluene is added into the sodium silicate solution, water is added into the solution for 3 hours after the solution is heated and reflowed at 130 ℃, the sodium silicate solution and the toluene are layered, the lower layer is the sodium silicate solution which has good fluidity (modulus is 2.2-2.8) and is colorless and transparent, and the upper layer toluene is recycled.
Example 4
And (3) burning the three wastes containing silicon at 1250+/-50 ℃ for 5 seconds to obtain solid-phase siliceous dust slag. Mixing the silicon-containing ash slag and 8% waste alkali liquor, heating at 100 ℃, stirring, and then introducing into a centrifuge for first centrifugal separation of solid and liquid phases; the liquid phase enters a stirring kettle, 27% of waste acid liquid is added into the stirring kettle to be stirred for 0.5h, sodium silicate is converted into solid-phase silicic acid, the liquid phase is discharged, and the solid-phase silicic acid is left in the stirring kettle; adding 7% of waste alkali liquor into a stirring kettle containing solid-phase silicic acid again to dissolve the silicic acid, and then repeating the process for 3 times by using 27% of waste acid and 7% of waste alkali liquor to convert sodium silicate into silicic acid and then sodium silicate; then toluene is added into the sodium silicate solution, water is added into the solution for 2 hours after the solution is heated and reflowed at 130 ℃, the sodium silicate solution and the toluene are layered, the lower layer is the sodium silicate solution with good fluidity (modulus is 2.8-3.2) and is colorless and transparent, and the upper layer toluene is recycled.
Comparative example 1
And (3) burning the three wastes containing silicon at 1000+/-50 ℃ for 3 seconds to obtain solid-phase siliceous dust slag. Mixing the silica-containing ash slag with 5% waste alkali liquor, stirring at 80 ℃ for 8 hours, and then introducing the mixture into a centrifuge for first centrifugal separation of solid and liquid phases; the liquid phase enters a stirring kettle, then toluene is added, water is added in the mixture after the mixture is heated and reflowed at 110 ℃ for 0.5h, the sodium silicate solution and the toluene are layered, the lower layer is the sodium silicate solution which has general fluidity (modulus is 3.1-3.8) and is dark brown, and the upper layer toluene is recycled.
Of course, the foregoing is merely preferred embodiments of the present invention and is not to be construed as limiting the scope of the embodiments of the present invention. The present invention is not limited to the above examples, and those skilled in the art will appreciate that the present invention is capable of equally varying and improving within the spirit and scope of the present invention.
Claims (5)
1. A method for preparing sodium silicate by using three organic silicon wastes in green recycling is characterized in that: the method comprises the following steps:
(1) Incinerating three wastes containing silicon to obtain solid-phase siliceous ash slag, wherein the three wastes containing silicon are three wastes generated by organosilicon monomer production enterprises;
(2) Mixing, heating and stirring the silicon-containing ash slag and the waste alkali liquid, and then centrifugally separating solid and liquid phases;
(3) The liquid phase enters a stirring kettle, waste acid liquid is added into the stirring kettle, sodium silicate is converted into solid-phase silicic acid, the liquid phase is discharged, and the solid-phase silicic acid is left in the stirring kettle;
(4) Adding waste alkali liquor into a stirring kettle containing solid-phase silicic acid, then adding toluene to heat with water for reflux, finely adjusting the modulus of sodium silicate solution, and separating and recovering;
the waste alkali liquid and the waste acid liquid are both generated in the production operation of the organic silicon chloromethane synthesis device.
2. The method for preparing sodium silicate by using three wastes of green recycled organic silicon according to claim 1, wherein the method comprises the following steps: in the three wastes containing silicon, waste gas is waste gas and exhaust gas generated from the upstream and downstream of an organosilicon monomer production enterprise; the waste solids are hydrolysate, slurry residue hydrolysate and semisolid sticky matters of the chloromethane synthesis device of the tail gas water washing system of the organic silicon monomer synthesis device; the waste liquid is slurry slag generated by synthesizing the organic silicon monomer, an organic silicon cracking kettle substrate, an azeotrope of the organic silicon monomer, an organic silicon disproportionation kettle substrate, methyl silicic acid generated by a comprehensive utilization device, water scrubber oily matters and alkaline residues.
3. The method for preparing sodium silicate by using three wastes of green recycled organic silicon according to claim 1, wherein the method comprises the following steps: the silicon-containing ash is SiO 2 The mass content of the incineration residue is more than 98.5 percent.
4. The method for preparing sodium silicate by using three wastes of green recycled organic silicon according to claim 1, wherein the method comprises the following steps: the alkali content in the waste alkali liquor is 5-8wt%; the HCl content in the waste acid liquid is 20-27wt%.
5. The method for preparing sodium silicate by using three wastes of green recycled organic silicon according to claim 1, wherein the method comprises the following steps: in the step (4), the water backflow time is 0.5-5h.
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| CN109678164A (en) * | 2018-12-25 | 2019-04-26 | 江西双龙硅材料科技有限公司 | A kind of environmentally protective white carbon black, caustic soda recycle combine production method |
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| US4973462A (en) * | 1987-05-25 | 1990-11-27 | Kawatetsu Mining Company, Ltd. | Process for producing high purity silica |
| CN101274763B (en) * | 2007-03-28 | 2012-09-05 | 万方 | Method for preparing layered sodium disilicate by using waste white slime and alkali waste water |
| CN102267857A (en) * | 2010-06-03 | 2011-12-07 | 中国林业科学研究院林产化学工业研究所 | Preparation method for nopadiene |
| CN102180472A (en) * | 2010-12-19 | 2011-09-14 | 何侠 | Method for preparing water glass and activated silica gel by using waste residues from treatment of sulfuric acid cinder |
| CN109737430A (en) * | 2019-01-03 | 2019-05-10 | 鲁西化工集团股份有限公司硅化工分公司 | A kind of hazardous waste processing system and method |
| KR102097728B1 (en) * | 2019-07-15 | 2020-04-06 | 에이엠나노텍 주식회사 | Method for Manufacturing Water Glass Using Rice Husk or Rice Husk Ash |
| CN113501529A (en) * | 2021-07-05 | 2021-10-15 | 安徽龙泉硅材料有限公司 | Preparation method of sodium silicate for tire reinforcing agent |
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| CN104876224A (en) * | 2015-05-11 | 2015-09-02 | 山东博润工业技术股份有限公司 | Organosilicon waste recovery treatment device and treatment method thereof |
| CN109678164A (en) * | 2018-12-25 | 2019-04-26 | 江西双龙硅材料科技有限公司 | A kind of environmentally protective white carbon black, caustic soda recycle combine production method |
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