CN104445221B - A kind of microwave-assisted rice hull ash prepares the new method of white carbon - Google Patents
A kind of microwave-assisted rice hull ash prepares the new method of white carbon Download PDFInfo
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- CN104445221B CN104445221B CN201410716518.5A CN201410716518A CN104445221B CN 104445221 B CN104445221 B CN 104445221B CN 201410716518 A CN201410716518 A CN 201410716518A CN 104445221 B CN104445221 B CN 104445221B
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Abstract
The present invention relates to chemical industry preparing technical field, a kind of method that microwave-assisted rice hull ash prepares high-performance white carbon, comprise the following steps: rice hull ash acidification, rice hull ash microwave basification, waterglass microwave modulus adjustment, acidizing product process.Compared with domestic existing alkaline-heating method, the concentration of reaction alkali liquor is substantially reduced, and the response time is greatly shortened, and on-demand can realize the adjustment of modulus of water glass；By microwave reaction, waterglass is carried out the adjustment of modulus, while greatly accelerating subsequent reactions neutrality condition, economizing on acid amount, the product quality of white carbon, increasing specific surface area can be effectively improved.The present invention response time is short, simple to operate, and more common rice hull ash is prepared white carbon black technique and more economized on acid, gentleer to the regularization condition of pH value, adapts to industrialized production and improves white carbon performance；Product separates thoroughly, purity is higher.
Description
Technical field
The present invention relates to fine inorganic chemical technology field, a kind of microwave-assisted rice hull ash prepares the new method of white carbon.
Background technology
Precipitated silica is a kind of superfine and active silicon dioxide granule, has another name called white carbon.Owing to it has special surface texture, special particle shape and the physicochemical property of uniqueness, it is widely used in the numerous areas such as rubber, plastics, coating, medicine and daily use chemicals.
At present, the production method of white carbon is mainly vapor phase method and the sedimentation method two kinds.The good characteristics such as product purity is high, dispersibility high although fume colloidal silica has, particle is thin and globulate, surface hydroxyl be few, but its raw materials used costliness, equipment requirements is high, technical sophistication, significantly limit its range of application.Precipitated silica currently mainly uses soda and silicon-containing material pyroreaction to prepare waterglass, adds strong acid reaction and prepares white carbon.Although the method products obtained therefrom activity is the highest, granule is wayward, and affinity is poor, but it is relatively low to the requirement of equipment, equipment is simple.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provides that energy consumption is little, is swift in response, the method realizing silicon dioxide high extraction by microwave reaction, and processed by the adjustment of the modulus to waterglass, can effectively reduce the difficulty of acid regulation pH value in subsequent technique, the product purity of final acquisition white carbon is higher, function admirable；Hydrochloric acid in course of reaction is regenerated, can effectively realize the recycling and reuse of hydrochloric acid, it is to avoid the waste of resource.
It is achieved particular by techniques below scheme:
A kind of microwave-assisted rice hull ash prepares the new method of white carbon, comprises the following steps:
(1) pretreatment: rice hull ash 1000g is crossed 80 ~ 100 mesh sieves, mixing according to the ratio that quality volume is 1:1 ~ 5 with the hydrochloric acid that concentration is 1% ~ 10%, stand 1 ~ 10h after stirring, then lotion is to neutral, rice hull ash is dried, and it is standby that filtrate regeneration obtains hydrochloric acid.
(2) rice hull ash microwave basification: the rice hull ash of step (1) isolated is mixed homogeneously according to the ratio that quality volume is 1:5 ~ 10 with the sodium hydroxide solution that concentration is 2% ~ 8%, is placed in tetrafluoroethene reactor carrying out microwave reaction；Separating gained mixed liquor, lotion is to neutral, it is thus achieved that water glass solution；
(3) waterglass microwave modulus adjustment: the water glass solution of step (2) is divided into solution a and solution b two parts according to certain volume ratio；By solution a addition deionized water, to be diluted to dioxide-containing silica be 1% ~ 5%, and drip regenerant salt acid solution in step (1) and occur to gel, and regulates PH=3 ~ 8；Solution b is adjusted to dioxide-containing silica be 3% ~ 10%；Above-mentioned two parts of solution mixing is placed in tetrafluoroethene reactor and carries out microwave reaction, it is thus achieved that modulus is the different water glass solutions of 1 ~ 3.5.
(4) acidifying obtains white carbon precipitation: add the surfactant of certain mass percent in the water glass solution that contained silicon dioxide quality mark is 15% ~ 30% obtained in step (3), after being sufficiently stirred for, it is incubated 60 DEG C ~ 80 DEG C, and drip the regeneration hydrochloric acid in certain density step (1), stirring is to stopped reaction during PH=8 ~ 10, still aging 1h ~ the 4h of system, separates and obtains white carbon.
(5) precipitation after lotion puts drying 2 ~ 4h under the conditions of 105 DEG C, obtains white carbon black product.
Further, in order to reduce energy consumption, it is ensured that response speed, reducing cost, improve product quality, in described pre-treatment step, the drying temperature of rice hull ash is 80 DEG C ~ 105 DEG C, and drying time is 2h ~ 6h.
Further, in order to reduce energy consumption, it is ensured that response speed, reducing cost, improve product quality, in described shell ash microwave basification step, the microwave reaction time is 5min-40min, and reaction power is 0.1kW ~ 0.5kW
Further, in order to ensure product quality, in described waterglass microwave modulus set-up procedure, the volume ratio of solution a with b is 1 ~ 3.5 to calculate and measure according to modulus of water glass, and its ratio is 1:1 ~ 7:1.
Further, in order to reduce energy consumption, it is ensured that response speed, in described waterglass microwave modulus set-up procedure, the microwave reaction time is 1min-10min, and reaction power is 0.05kW ~ 0.2kW.
Further, in order to ensure product quality, described acidifying obtains in white carbon settling step, described surfactant addition is water glass solution quality 0.1% ~ 0.5%, its activating agent is EDTA, PEG-4000 one or more.
Further, reducing cost, in order to ensure product quality, described acidifying obtains in white carbon settling step, and concentration of hydrochloric acid is 2mol/L ~ 4mol/L.
The technique effect of the present invention is embodied in: compared with preparing white carbon black technique with domestic existing rice hull ash soda boiling, and the concentration of reaction alkali liquor is substantially reduced, and the response time is greatly shortened, and on-demand can realize the adjustment of modulus of water glass；By microwave reaction, waterglass is carried out the adjustment of modulus, while greatly accelerating subsequent reactions neutrality condition, economizing on acid amount, the product quality of white carbon, increasing specific surface area can be effectively improved, be suitable for industrialized production.
Accompanying drawing explanation
Fig. 1 is the process chart that the microwave-assisted rice hull ash of the present invention prepares the new method of white carbon.
Detailed description of the invention
Below in conjunction with specific embodiment and accompanying drawing, technical scheme is further elaborated, but claimed scope is not only limited to description.
Embodiment one
As it is shown in figure 1, a kind of microwave-assisted rice hull ash prepares the new method of white carbon, comprise the following steps:
(1) pretreatment: rice hull ash 1000g is crossed 80 mesh sieves, then mixes according to the ratio that mass volume ratio is 1:3 with the hydrochloric acid that concentration is 3%, stands 3h after stirring, then lotion is to neutral, rice hull ash is dried, and it is standby that filtrate regeneration obtains hydrochloric acid solution.
(2) rice hull ash microwave basification: the rice hull ash of step (1) isolated is mixed homogeneously according to the ratio that mass volume ratio is 1:10 with the sodium hydroxide solution that concentration is 3%, it is placed in tetrafluoroethene reactor carrying out microwave reaction, response time is 30min, and reaction power is 0.4kW；Separating gained mixed liquor, lotion is to neutral, it is thus achieved that water glass solution；
(3) waterglass microwave modulus adjustment: the water glass solution produced in step (2) is divided into solution a and solution b two parts；Solution a is added deionized water, and to be diluted to silicon dioxide quality mark be 2%, and drip the hydrochloric acid solution that step (1) regenerates and occur to gel, and regulates PH=6；Solution b heating is concentrated into silicon dioxide quality mark is 10%；Two parts of solution after processing are mixed in tetrafluoroethene reactor and carry out microwave reaction, and the response time is 5min, and reaction power is 0.2kW.
(4) acidifying obtains white carbon precipitation: adding mass percentage content in the water glass solution obtained in step (3) is the surfactant of 0.1%, after being sufficiently stirred for, it is incubated 80 DEG C, and drip the hydrochloric acid solution of 2mol/L, stopped reaction when continuing stirring until PH=9.5, the still aging 4h of system, separates and obtains white carbon.
(5) precipitation after lotion is as drying 4h in 105 DEG C of baking ovens, obtains white carbon black product.
Embodiment two
As it is shown in figure 1, a kind of microwave-assisted rice hull ash prepares the new method of white carbon, comprise the following steps:
(1) pretreatment: rice hull ash 1000g is crossed 80 mesh sieves, mixes according to the ratio that quality volume is 1:5 with the hydrochloric acid that concentration is 1%, stands 10h after stirring, and then lotion is to neutral, rice hull ash is dried, and it is standby that filtrate regeneration obtains hydrochloric acid solution.
(2) rice hull ash microwave basification: the rice hull ash of step (1) isolated is mixed homogeneously according to the ratio that mass volume ratio is 1:8 with the sodium hydroxide solution that concentration is 4%, it is placed in tetrafluoroethene reactor carrying out microwave reaction, response time is 20min, and reaction power is 0.35kW；Mixed liquor is separated, and lotion is to neutral, it is thus achieved that water glass solution；
(3) waterglass microwave modulus adjustment: gained water glass solution in step (2) is divided into solution a and solution b two parts；Add deionized water being diluted to dioxide-containing silica to solution a is 3%, and the regenerant salt acid solution dripping step (1) occurs to gel, and regulates PH=7；Solution b heating is concentrated into dioxide-containing silica is 8%；Two parts of solution after processing are mixed in tetrafluoroethene reactor and carry out microwave reaction, and the response time is 8min, and reaction power is 0.1kW.
(4) acidifying obtains white carbon precipitation: adding mass percentage content in the water glass solution obtained in step (3) is the surfactant of 0.3%, after being sufficiently stirred for, insulation is 80 DEG C, and drip the hydrochloric acid solution of 3mol/L, stopped reaction when continuing stirring until PH=8.5, the still aging 2h of system, separates and obtains white carbon.
(5) precipitation after lotion is as drying 3h in 105 DEG C of baking ovens, obtains white carbon black product.
Embodiment three
As it is shown in figure 1, a kind of microwave-assisted rice hull ash prepares the new method of white carbon, comprise the following steps:
(1) pretreatment: rice hull ash 1000g is crossed 100 mesh sieves, then mixes according to the ratio that quality volume is 1:1 with the hydrochloric acid that concentration is 5%, stands 1h after stirring, then lotion is to neutral, rice hull ash is dried, and it is standby that filtrate regeneration obtains hydrochloric acid solution.
(2) rice hull ash microwave basification: the rice hull ash of step (1) isolated is mixed homogeneously according to the ratio that quality volume is 1:5 with the sodium hydroxide solution that concentration is 8%, it is placed in tetrafluoroethene reactor carrying out microwave reaction, response time is 10min, and reaction power is 0.2kW；Gained mixed liquor is separated, and lotion is to neutral, it is thus achieved that certain density water glass solution；
(3) waterglass microwave modulus adjustment: the water glass solution produced in step (2) is divided into solution a and solution b two parts；Solution a is added deionized water, and to be diluted to dioxide-containing silica be 5%, and drip the hydrochloric acid solution that step (1) regenerates and occur to gel, and regulates PH=8；Solution b heating is concentrated into dioxide-containing silica is 9%；Two parts of solution mixing after processing are placed in tetrafluoroethene reactor carrying out microwave reaction, and the response time is 10min, and reaction power is 0.15kW.
(4) acidifying obtains white carbon precipitation: adding mass percentage content in the water glass solution obtained in step (3) is the surfactant of 0.5%, after being sufficiently stirred for, insulation is 80 DEG C, and drip the hydrochloric acid solution of 4mol/L, stopped reaction when continuing stirring until PH=8, the still aging 1h of system, separates and obtains white carbon.
(5) precipitation after lotion is as drying 2.5h in 105 DEG C of baking ovens, obtains white carbon black product.
Claims (7)
1. a microwave-assisted rice hull ash prepares the new method of white carbon, it is characterised in that comprise the following steps:
(1) pretreatment: rice hull ash 1000g is crossed 80-100 mesh sieve, mixing according to the ratio that quality volume is 1:1 ~ 5 with the hydrochloric acid that concentration is 1% ~ 10%, stand 1 ~ 10h after stirring, then lotion is to neutral, rice hull ash is dried, and it is standby that filtrate regeneration obtains hydrochloric acid；(2) rice hull ash microwave basification: the rice hull ash of step (1) isolated is mixed homogeneously according to the ratio that mass volume ratio is 1:5 ~ 10 with the sodium hydroxide solution that concentration is 2%-8%, is placed in tetrafluoroethene reactor carrying out microwave reaction；Separating gained mixed liquor, lotion is to neutral, it is thus achieved that water glass solution；
(3) waterglass microwave modulus adjustment: the water glass solution of step (2) is divided into solution a and solution b two parts according to certain volume ratio；Solution a addition deionized water is diluted to dioxide-containing silica is 1% ~ 5%, and the regenerant salt acid solution dripped in step (1) occurs to gel, regulates PH=3 ~ 8；Solution b is adjusted to dioxide-containing silica be 3% ~ 10%；Above-mentioned two parts of solution mixing is placed in tetrafluoroethene reactor carrying out microwave reaction, it is thus achieved that modulus is the different water glass solutions of 1 ~ 3.5；(4) acidifying obtains white carbon precipitation: add the surfactant of certain mass percent in the water glass solution that contained silicon dioxide quality mark is 15% ~ 30% obtained in step (3), after being sufficiently stirred for, it is incubated 60 DEG C ~ 80 DEG C, and drip the regeneration hydrochloric acid in certain density step (1), stir to stopping dropping during reaction terminating PH=8 ~ 10, still aging 1h ~ the 4h of system, separates and obtains white carbon；(5) precipitation after lotion puts drying 2 ~ 4h under the conditions of 105 DEG C, obtains white carbon black product.
2. microwave-assisted rice hull ash as claimed in claim 1 prepares the new method of white carbon, it is characterised in that: in described pre-treatment step, the drying temperature of rice hull ash is 80 DEG C ~ 105 DEG C, and drying time is 2h ~ 6h.
3. microwave-assisted rice hull ash as claimed in claim 1 prepares the new method of white carbon, it is characterised in that: in described rice hull ash microwave basification step, the microwave reaction time is 5min ~ 40min, and reaction power is 0.1kW ~ 0.5kW.
4. microwave-assisted rice hull ash as claimed in claim 1 prepares the new method of white carbon, it is characterized in that: in described waterglass microwave modulus set-up procedure, the volume ratio of solution a with b is 1 ~ 3.5 to calculate and measure according to modulus of water glass, and its ratio is 1:1 ~ 7:1.
5. microwave-assisted rice hull ash as claimed in claim 1 prepares the new method of white carbon, it is characterised in that: in described waterglass microwave modulus set-up procedure, the microwave reaction time is 1min-10min, and reaction power is 0.05kW ~ 0.2kW.
6. microwave-assisted rice hull ash as claimed in claim 1 prepares the new method of white carbon, it is characterized in that: described acidifying obtains in white carbon settling step, described surfactant addition is water glass solution quality 0.1% ~ 0.5%, its activating agent elect as EDTA, PEG-4000 one or more.
7. microwave-assisted rice hull ash as claimed in claim 1 prepares the new method of white carbon, it is characterised in that: described acidifying obtains in white carbon settling step, and concentration of hydrochloric acid is 2mol/L ~ 4mol/L.
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| CN107697920A (en) * | 2017-11-21 | 2018-02-16 | 安徽伊法拉电气有限公司 | A kind of method that hydrophobic nano white carbon is prepared using sol-gal process |
| CN109467094A (en) * | 2018-12-25 | 2019-03-15 | 安徽确成硅化学有限公司 | A kind of preparation method preparing functional white carbon black using the leaf of bamboo |
| CN112357927B (en) * | 2020-09-30 | 2022-12-02 | 北京市政建设集团有限责任公司 | Organic-inorganic composite water glass and preparation method thereof |
| CN113200551A (en) * | 2021-04-29 | 2021-08-03 | 武汉理工大学 | Preparation method of modified white carbon black |
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| CN103803558A (en) * | 2013-12-20 | 2014-05-21 | 浙江中天氟硅材料有限公司 | Method for preparing precipitation-method white carbon black by utilizing organosilicon dust-containing tail gas hydrolysate |
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Effective date of registration: 20191128 Address after: Datun Zhongjia, Dalong Economic Development Zone, Tongren City, Guizhou Province 550000 Patentee after: GUIZHOU DALONGYISHOU VEGETABLE OIL CO., LTD. Address before: 561011 Guizhou province Tongren area water Bijiang District of Tongren City Road No. 103 Patentee before: tongren university |
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