CN117208915A - High-purity optical coated silicon dioxide and preparation method thereof - Google Patents

High-purity optical coated silicon dioxide and preparation method thereof Download PDF

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Publication number
CN117208915A
CN117208915A CN202310987694.1A CN202310987694A CN117208915A CN 117208915 A CN117208915 A CN 117208915A CN 202310987694 A CN202310987694 A CN 202310987694A CN 117208915 A CN117208915 A CN 117208915A
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silica
silicon dioxide
powder
grinding
purity
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蔡沐之
蔡轩臣
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Jiangsu Dongfang Shuohua Optical Material Co ltd
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Jiangsu Dongfang Shuohua Optical Material Co ltd
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Abstract

The invention provides high-purity optical coated silica, and a preparation method of the high-purity optical coated silica, which comprises the following specific preparation steps: s1: mechanical crushing treatment of a silicon dioxide raw material, and S2: silica separation reaction extraction treatment, S3: sintering treatment of silica precipitate, S4: silica spin cleaning treatment, S5: drying the silicon dioxide powder, S6: purifying silicon dioxide powder, S7: the preparation method of the optical coating silicon dioxide designed by the invention can effectively improve the refractive index and the light transmittance of the optical coating finished product so as to ensure the yield of the optical coating finished product.

Description

High-purity optical coated silicon dioxide and preparation method thereof
Technical Field
The invention relates to the technical field of silicon dioxide preparation, in particular to high-purity optical coated silicon dioxide and a preparation method thereof.
Background
Silica, which is an inorganic compound of the formula SiO2, silicon atoms and oxygen atoms are arranged in long range order to form crystalline silica, short range order or long range order to form amorphous silica, in which the silicon atoms are located at the center of a regular tetrahedron, four oxygen atoms are located at the four vertices of the regular tetrahedron, a number of such tetrahedrons are connected by the oxygen atoms of the vertices, each oxygen atom being shared by two tetrahedrons, i.e. each oxygen atom is bonded to two silicon atoms, the simplest formula of silica is SiO2, but SiO2 does not represent a simple molecule (only represents the ratio of the number of atoms of silicon and oxygen in the silica crystal). Pure natural silica crystals, which are a solid, colorless transparent, hard, brittle, insoluble, and commonly used in the manufacture of optical instruments and the like, silica is used for optical coating, the manufacture of flat glass, glass products, foundry sand, glass fibers, ceramic colored glazes, sand blasting for rust prevention, sand for filtration, fluxes, refractory materials, and the manufacture of lightweight bubble concrete. Can be used for manufacturing important parts, optical instruments and artworks in the electronic industry, and is an important raw material for manufacturing optical fibers. Rubber synthesis reinforcing materials, synthetic resin fillers, ink (ink-jet printer), paint thickeners, matting agents, feed additives, quartz glass and glass cement production, but the purity requirements of silicon dioxide for optical coating are high, and high-purity extraction treatment is required for the silicon dioxide raw materials.
However, the existing purification preparation method of high-purity optical coated silica has the following problems: when the silicon dioxide prepared in the prior art is used for optical coating, the obtained product has poor compactness due to the large internal aperture and uneven internal structure distribution, and the refractive index and the light transmittance of the coating are influenced, so that the yield of the optical coating is influenced. For this purpose, a corresponding technical solution is required to be designed to solve the existing technical problems.
Disclosure of Invention
The invention aims to provide high-purity optical coating silicon dioxide and a preparation method thereof, which solve the technical problems that when the silicon dioxide prepared in the prior art is used for optical coating, the obtained product has poor compactness due to larger internal aperture and uneven internal structure distribution, and the refractive index and the light transmittance of the coating are influenced, so that the yield of the optical coating is influenced.
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method of the high-purity optical coated silica comprises the following specific preparation steps:
s1: mechanically crushing the silicon dioxide raw material;
s2: silica separation reaction and extraction treatment;
s3: sintering the silica precipitate;
s4: silica rotary cleaning treatment;
s5: drying silicon dioxide powder;
s6: purifying silicon dioxide powder;
s7: grinding and refining the silicon dioxide micro powder;
through the seven steps, the silicon dioxide can be subjected to sequential raw material mechanical crushing, separation reaction extraction, sediment sintering, rotary cleaning, powder drying, powder purification and micro powder grinding refinement, so that the high purity of the silicon dioxide and the fineness of the silicon dioxide are improved.
As a preferred embodiment of the present invention, S1: the method comprises the steps of mechanically crushing a silicon dioxide raw material, introducing the silicon dioxide raw material quartz stone into a crusher for crushing, grinding quartz sand into quartz sand through a grinding mechanism, and grinding the quartz sand into quartz particles with diameters of 2mm-5mm for later use.
As a preferred embodiment of the present invention, S2: the silica is separated, reacted and extracted, and the silica powder is prepared through mixing silica sand, water, structure guiding agent, alkali or acid in certain proportion, sealing inside pressure resisting reaction kettle, heating to 150-250 deg.c, maintaining the temperature for 5-12 hr, cooling the reaction kettle, washing the reacted product with water or dilute acid to pH 8-11, and stoving.
As a preferred embodiment of the present invention, S3: the silica precipitate sintering treatment comprises introducing raw silica powder into a heating vessel, sintering at 800-1450 ℃, and heating and melting the silica powder obtained in the sintering step at a temperature of 2000-2000 ℃ to the boiling point of silica in a plasma torch in which argon gas is introduced at a predetermined flow rate and plasma is generated at a predetermined high-frequency output power by a thermal plasma spheroidizing step.
As a preferred embodiment of the present invention, S4: and (3) a silica rotary cleaning treatment, namely introducing the silica powder into a cleaning container, and removing micro powder attached to the surface of the spheroidized silica powder for standby.
As a preferred embodiment of the present invention, S5: and (3) drying the silicon dioxide powder, and introducing the silicon dioxide micro powder into a tube furnace for roasting and activating treatment.
As a preferred embodiment of the present invention, S6: and (3) purifying the silicon dioxide powder, namely mixing the dried silicon dioxide micro powder and HCL gas into silicon trichloride with a relatively low boiling point in a reactor, purifying by adopting a chemical reaction equation of Si+3HCl=SiHCl < 3+ > H2, then purifying by distillation at a high temperature, and removing hydrogen to obtain the high-purity silicon dioxide micro powder.
As a preferred embodiment of the present invention, S7: grinding and refining the silicon dioxide micropowder, putting the purified silicon dioxide micropowder into a high-precision grinding container, and grinding the silicon dioxide to powder with the diameter of 0.3-0.6 mm by a repeated grinding mode.
Compared with the prior art, the invention has the following beneficial effects:
1. the scheme designs a preparation method of high-purity optical coated silica, which comprises the steps of mechanical crushing, separation reaction extraction, sediment sintering, rotary cleaning, powder drying, powder purification and micro powder grinding and refinement, wherein the seven steps can achieve the purification of the silica and the improvement of the fineness of the silica, in the process of the sintering treatment of the sediment of the silica, the thermal plasma spheroidization procedure is utilized, the silica powder obtained in the sintering procedure is input into a plasma torch which introduces argon at a preset flow rate and generates plasma at a preset high-frequency output power at a preset supply speed, the purity of the silica can be greatly improved by the produced silica sealing film, the subsequent powder purification treatment, the distillation and the high-temperature purification are adopted, the hydrogen is removed, the high-purity silica micro powder is obtained, and in addition, the repeated grinding mode can be adopted to improve the grinding and refinement of the silica micro powder so as to ensure the refractive index and the light transmittance of the silica coating.
2. The preparation method of the optical coating silicon dioxide can effectively improve the refractive index and the light transmittance of the optical coating finished product so as to ensure the yield of the optical coating finished product.
Detailed Description
Example 1:
the preparation method of the high-purity optical coated silica comprises the following specific preparation steps:
s1: mechanically crushing the silicon dioxide raw material;
s2: silica separation reaction and extraction treatment;
s3: sintering the silica precipitate;
s4: silica rotary cleaning treatment;
s5: drying silicon dioxide powder;
s6: purifying silicon dioxide powder;
s7: grinding and refining the silicon dioxide micro powder;
through the seven steps, the silicon dioxide can be subjected to sequential raw material mechanical crushing, separation reaction extraction, sediment sintering, rotary cleaning, powder drying, powder purification and micro powder grinding refinement, so that the high purity of the silicon dioxide and the fineness of the silicon dioxide are improved.
S1: the method comprises the steps of mechanically crushing a silicon dioxide raw material, introducing the silicon dioxide raw material quartz stone into a crusher for crushing, grinding quartz sand into quartz sand through a grinding mechanism, and grinding the quartz sand into quartz particles with the diameter of 3mm for later use.
S2: the silica is separated, reacted and extracted, and the silica powder is prepared through mixing silica sand, water, structure guiding agent, alkali or acid in certain proportion, sealing inside pressure resisting reaction kettle, heating to 200 deg.c, maintaining the temperature for 9 hr, cooling the reaction kettle, washing the reaction product with water or dilute acid to pH of 10 and stoving.
S3: the silica precipitate sintering treatment comprises introducing raw silica powder into a heating vessel, sintering at 1100 ℃, and heating and melting the silica powder obtained in the sintering step at a temperature of 2000 ℃ to the boiling point of silica in a plasma torch in which argon gas is introduced at a predetermined flow rate and plasma is generated at a predetermined high-frequency output by a thermal plasma spheroidizing step.
S4: and (3) a silica rotary cleaning treatment, namely introducing the silica powder into a cleaning container, and removing micro powder attached to the surface of the spheroidized silica powder for standby.
S5: and (3) drying the silicon dioxide powder, and introducing the silicon dioxide micro powder into a tube furnace for roasting and activating treatment.
S6: and (3) purifying the silicon dioxide powder, namely mixing the dried silicon dioxide micro powder and HCL gas into silicon trichloride with a relatively low boiling point in a reactor, purifying by adopting a chemical reaction equation of Si+3HCl=SiHCl < 3+ > H2, then purifying by distillation at a high temperature, and removing hydrogen to obtain the high-purity silicon dioxide micro powder.
S7: grinding and refining the silica micropowder, putting the purified silica micropowder into a high-precision grinding container, and grinding the silica to powder with the diameter of 0.5mm by a repeated grinding mode.
The scheme designs a preparation method of high-purity optical coated silica, which comprises the steps of mechanical crushing, separation reaction extraction, sediment sintering, rotary cleaning, powder drying, powder purification and micro powder grinding and refinement, wherein the seven steps can achieve the purification of the silica and the improvement of the fineness of the silica, in the process of the sintering treatment of the sediment of the silica, the spheroidization procedure of thermal plasma is utilized, the silica powder obtained in the sintering procedure is put into a plasma torch which is used for introducing argon at a preset flow rate and generating plasma at a preset high-frequency output power at a preset supply speed, the purity of the silica can be greatly improved by the produced silica sealing film, the subsequent powder purification treatment is adopted, the distillation and the high-temperature purification are adopted, the hydrogen is removed, the high-purity silica micro powder is obtained, in addition, the repeated grinding mode is adopted, the grinding and refinement of the silica micro powder can be improved, the refractive index and the light transmittance of the silica coating film are ensured, and the refractive index and the light transmittance of the finished optical coating film can be effectively improved, and the yield of the optical coating film is ensured.
Example 2:
the preparation method of the high-purity optical coated silica comprises the following specific preparation steps:
s1: mechanically crushing the silicon dioxide raw material;
s2: silica separation reaction and extraction treatment;
s3: sintering the silica precipitate;
s4: silica rotary cleaning treatment;
s5: drying silicon dioxide powder;
through the five steps, the silicon dioxide can be subjected to sequential raw material mechanical crushing, separation reaction extraction, sediment sintering, rotary cleaning and powder drying, so that the purity of the silicon dioxide is improved.
S1: the method comprises the steps of mechanically crushing a silicon dioxide raw material, introducing the silicon dioxide raw material quartz stone into a crusher for crushing, grinding quartz sand into quartz sand through a grinding mechanism, and grinding the quartz sand into quartz particles with the diameter of 3mm for later use.
S2: the silica is separated, reacted and extracted, and the silica powder is prepared through mixing silica sand, water, structure guiding agent, alkali or acid in certain proportion, sealing inside pressure resisting reaction kettle, heating to 200 deg.c, maintaining the temperature for 9 hr, cooling the reaction kettle, washing the reaction product with water or dilute acid to pH of 10 and stoving.
S3: the silica precipitate sintering treatment comprises introducing raw silica powder into a heating vessel, sintering at 1100 ℃, and heating and melting the silica powder obtained in the sintering step at a temperature of 2000 ℃ to the boiling point of silica in a plasma torch in which argon gas is introduced at a predetermined flow rate and plasma is generated at a predetermined high-frequency output by a thermal plasma spheroidizing step.
S4: and (3) a silica rotary cleaning treatment, namely introducing the silica powder into a cleaning container, and removing micro powder attached to the surface of the spheroidized silica powder for standby.
S5: and (3) drying the silicon dioxide powder, and introducing the silicon dioxide micro powder into a tube furnace for roasting and activating treatment.
The scheme designs a preparation method of high-purity optical coated silica, which comprises the steps of mechanical crushing, separation reaction extraction, sediment sintering, rotary cleaning, powder drying, powder purification and micro powder grinding and refinement, wherein the seven steps can achieve the purification of the silica and the improvement of the fineness of the silica, and in the process of the sintering treatment of the silica sediment, the high-purity silica micro powder is obtained by introducing argon into a plasma torch for generating plasma at a preset flow rate and a preset high-frequency output power in a preset feeding speed in a process of spheroidizing the silica sediment by utilizing a thermal plasma, so that the purity of the silica can be greatly improved by adopting the powder purification treatment, and the purification is carried out at a high temperature by adopting distillation to remove hydrogen.
Specifically, the optical coating silicon dioxide is purified according to the production and preparation modes of the two groups of examples, and 1000kg of quartz stone is taken as a raw material for purifying the silicon dioxide in each example to prepare an optical coating, and the specific steps are as follows:
experimental group Quartz raw material/kg Purification rate/% Refractive index of optical coating film Optical coating film light transmittance
Example 1 1000 53.8 3.5 93
Example 2 1000 42.6 2.1 83.5
In addition, as can be seen from the above comparison parameters, the existing silica sand purification steps are optimized, and the purification of silica and the improvement of the fineness of silica can be achieved through mechanical crushing, separation reaction extraction, sediment sintering, rotary cleaning, powder drying, powder purification and micropowder grinding refinement, wherein in the process of the silica sediment sintering treatment, the refractive index and the transmittance of the optical coating film finished product can be effectively improved by using a thermal plasma spheroidizing procedure, in a plasma torch which introduces argon into a predetermined flow and generates plasma with a predetermined high-frequency output power, and the silica powder obtained in the sintering procedure is fed into the plasma torch with a predetermined feeding speed, so that the produced silica sealing film can greatly improve the purity of the silica, and the purification of the silica micropowder with high purity can be achieved by adopting distillation and high-temperature purification to remove hydrogen.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. A preparation method of high-purity optical coated silica is characterized by comprising the following steps: the preparation method comprises the following specific steps:
s1: mechanically crushing the silicon dioxide raw material;
s2: silica separation reaction and extraction treatment;
s3: sintering the silica precipitate;
s4: silica rotary cleaning treatment;
s5: drying silicon dioxide powder;
s6: purifying silicon dioxide powder;
s7: grinding and refining the silicon dioxide micro powder;
through the seven steps, the silicon dioxide can be subjected to sequential raw material mechanical crushing, separation reaction extraction, sediment sintering, rotary cleaning, powder drying, powder purification and micro powder grinding refinement, so that the high purity of the silicon dioxide and the fineness of the silicon dioxide are improved.
2. The method for preparing high-purity optical coated silica according to claim 1, wherein: s1: the method comprises the steps of mechanically crushing a silicon dioxide raw material, introducing the silicon dioxide raw material quartz stone into a crusher for crushing, grinding quartz sand into quartz sand through a grinding mechanism, and grinding the quartz sand into quartz particles with diameters of 2mm-5mm for later use.
3. The method for preparing high-purity optical coated silica according to claim 1, wherein: s2: the silica is separated, reacted and extracted, and the silica powder is prepared through mixing silica sand, water, structure guiding agent, alkali or acid in certain proportion, sealing inside pressure resisting reaction kettle, heating to 150-250 deg.c, maintaining the temperature for 5-12 hr, cooling the reaction kettle, washing the reacted product with water or dilute acid to pH 8-11, and stoving.
4. The method for preparing high-purity optical coated silica according to claim 1, wherein: s3: the silica precipitate sintering treatment comprises introducing raw silica powder into a heating vessel, sintering at 800-1450 ℃, and heating and melting the silica powder obtained in the sintering step at a temperature of 2000-2000 ℃ to the boiling point of silica in a plasma torch in which argon gas is introduced at a predetermined flow rate and plasma is generated at a predetermined high-frequency output power by a thermal plasma spheroidizing step.
5. The high-purity optical coated silica according to claim 1, wherein: s4: and (3) a silica rotary cleaning treatment, namely introducing the silica powder into a cleaning container, and removing micro powder attached to the surface of the spheroidized silica powder for standby.
6. The method for preparing high-purity optical coated silica according to claim 1, wherein: s5: and (3) drying the silicon dioxide powder, and introducing the silicon dioxide micro powder into a tube furnace for roasting and activating treatment.
7. The method for preparing high-purity optical coated silica according to claim 1, wherein: s6: and (3) purifying the silicon dioxide powder, namely mixing the dried silicon dioxide micro powder and HCL gas into silicon trichloride with a relatively low boiling point in a reactor, purifying by adopting a chemical reaction equation of Si+3HCl=SiHCl < 3+ > H2, then purifying by distillation at a high temperature, and removing hydrogen to obtain the high-purity silicon dioxide micro powder.
8. The method for preparing high-purity optical coated silica according to claim 1, wherein: s7: grinding and refining the silicon dioxide micropowder, putting the purified silicon dioxide micropowder into a high-precision grinding container, and grinding the silicon dioxide to powder with the diameter of 0.3-0.6 mm by a repeated grinding mode.
CN202310987694.1A 2023-08-08 2023-08-08 High-purity optical coated silicon dioxide and preparation method thereof Pending CN117208915A (en)

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CN202310987694.1A CN117208915A (en) 2023-08-08 2023-08-08 High-purity optical coated silicon dioxide and preparation method thereof

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Application Number Priority Date Filing Date Title
CN202310987694.1A CN117208915A (en) 2023-08-08 2023-08-08 High-purity optical coated silicon dioxide and preparation method thereof

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CN117208915A true CN117208915A (en) 2023-12-12

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