CN106370553A - Method for detecting solid content of slurry - Google Patents
Method for detecting solid content of slurry Download PDFInfo
- Publication number
- CN106370553A CN106370553A CN201611004758.8A CN201611004758A CN106370553A CN 106370553 A CN106370553 A CN 106370553A CN 201611004758 A CN201611004758 A CN 201611004758A CN 106370553 A CN106370553 A CN 106370553A
- Authority
- CN
- China
- Prior art keywords
- slurry
- solid content
- chlorosilane
- detection method
- centrifuge
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method for detecting the solid content of slurry so as to overcome the defects in the prior art. The method comprises the following steps: a, performing centrifugal treatment on a stirred chlorosilane slurry sample by a centrifugal machine; b, purging the residual volatile chlorosilane liquid by introducing nitrogen; and c, weighing the weight of the residual solid to obtain the solid content of the slurry. According to the method for detecting the solid content of the chlorosilane slurry in a cold hydrogenation process provided by the invention, the chlorosilane slurry and the chlorosilane liquid are separated by the centrifugal machine and then are treated, so the detection time is greatly shortened. The detection method is simple and convenient to operate, clean, safe and insusceptible to environmental pollution; furthermore, a polytetrafluoroethylene centrifugal test tube is insusceptible to corrosion, and cleaning and maintenance of appliances, such as the centrifugal test tube and the like, are facilitated after detection is finished.
Description
Technical field
The invention belongs to production of polysilicon detection field, more particularly, to a kind of inflammable, explosive, highly volatile, corrosivity are strong
And the detection method of the solid mixed material chemicals slurry solid content of liquid to moisture-sensitive.
Background technology
Traditional Siemens Method produces in polysilicon process, and product per ton wants more than 20 ton of Silicon chloride. of by-product, substantial amounts
Side-product constrain polysilicon extensive development, silicon tetrachloride cold hydrogenation technology solves this problem, Silicon chloride. is turned
Turn to trichlorosilane to use as feedstock circulation, therefore larger ton polycrystalline silicon device occurs one after another.But it is existing
Cold hydrogenation technology still have imperfection in place of, exist many problems have to be solved, wherein in production process the discharge of slurry and
Process is concern instantly, due to impurity such as the remaining silica flour in system in whole production process, aluminum chloride, ferric chlorides
Presence, system jams, equipment attrition can be led to, impact is normal to be run.For this problem, mainly take regular or indefinite at present
Phase discharges the method for some materials to reduce the impurity content in apparatus system, and is protected by constantly discharging more material
Hold the impurity in system and maintain a maintenance level.So not only cause material consumption to increase, and slurry treating capacity also accordingly increases
Add, bring bigger pressure to downstream environmental protection treatment program.For this reason, the slurry that this cold hydrogenation reactor outlet produces need to be contained
Gu amount is detected and is taken the measure of being correspondingly improved.A kind of polycrystalline is disclosed in the patent of Patent No. cn20111033040
Silicon produce in waste gas and liquids treatment method, but the method just for waste gas and waste liquid in production of polysilicon process it is impossible to use for reference
Detection method for solid content in slurry.
A kind of mensure of concrete mixing plant waste slurry solid content is disclosed in the patent of Patent No. cn105547905a
Device and method, the method is related to construction material test equipment technical field, is measured using mechanical type method, and detection process needs
Drying, constant weight, process are loaded down with trivial details, detection time is longer, and contain chlorosilane in slurry, low boiling point, and heating is inflammable and explosive (mainly several
The boiling point planting chlorosilane is all than relatively low), the step of drying is not suitable for the process of chlorosilane slurry.
Content of the invention
The problem that the present invention solves is that chlorosilane slurry centrifuge in cold hydrogenation process is carried out centrifugal treating, then will starch
The chlorosilane nitrogen being mixed with material dries up, and is weighed after re-dry, and dried sample mass accounts for the matter of original sample quality
, as the solid content of slurry, the method detection time is short for amount fraction, have easy and simple to handle, clean, safely, be difficult to pollute environment,
And polytetrafluoro centrifuge tube is not perishable, the clean and maintenance of the utensils such as centrifuge tube is easy in detection after terminating.
In order to solve the above problems, a kind of detection method of slurry solid content provided by the present invention is it is characterised in that wrap
Include following steps: a. to take a certain amount of slurry and weigh；B. agitated chlorosilane slurry sample is carried out at centrifugation with centrifuge
Reason；C. it is passed through nitrogen and purge out remaining volatile chlorosilane liquid produced；D. weigh up the quality of remaining solid, draw containing in slurry
Gu amount.
Wherein:
In step b: agitated chlorosilane slurry sample be placed in be pre-dried and weighed polytetrafluoro centrifuge tube in,
Place into and in centrifuge, carry out centrifugal treating.
In step c: centrifuge tube and nitrogen pipeline are connected by effusion meter, then carries out nitrogen purging.
In step b: described centrifuge tube is made up of corrosion-resistant material.
In one preferably or alternatively embodiment, the rotating speed of centrifuge is 3000r/min, and the time of centrifugal treating is
3min.
In one preferably or alternatively embodiment, the centrifuge tube of polytetrafluoro carries purging function.
In one preferably or alternatively embodiment, effusion meter flow is 1.6l/min.
In one preferably or alternatively embodiment, nitrogen purge time is 10min.
The invention has the beneficial effects as follows, located again after chlorosilane slurry and chlorosilane liquid produced centrifuge are carried out separating
Reason, substantially reduces detection time, this detection method have easy and simple to handle, clean, safely, be difficult to pollute environment, and polytetrafluoro
Centrifuge tube is not perishable, and the clean and maintenance of the utensils such as centrifuge tube is easy in detection after terminating.
In addition, the optimal technical scheme that the present invention provides compared with prior art at least can also produce following technology
Effect: experimental data shows, effusion meter flow is 1.6l/min, and nitrogen purge time is 10min, purges best results.
With reference to embodiment, the present invention is further described.
Specific embodiment
A kind of slurry solid content detection method, comprises the following steps: a. takes a certain amount of chlorosilane slurry sample and weighs；
B. agitated chlorosilane slurry sample carries out centrifugal treating with centrifuge；C. be passed through nitrogen purge out remaining volatile
Chlorosilane liquid produced；D. weigh up the quality of remaining solid, draw the solid content in slurry.
During detection: 1. the chlorosilane slurry sample (chlorosilane slurry mixed liquor 30ml) of stirring of learning from else's experience is placed in and is pre-dried simultaneously
In the polytetrafluoro centrifuge tube that weighing (title standard to 0.02g) is crossed, add a cover rapidly, weigh (title standard to 0.02g), draw sample mass
m0.
2. chlorosilane slurry sample is put into 3000r/min centrifugal treating 3min in centrifuge, centrifugation will be upper after finishing
Layer empties in waste liquid bottle.
3. by entering nitrogen after being attached polytetrafluoro centrifuge tube by effusion meter and nitrogen pipeline, with nitrogen flow
Weigh (through test, selecting the 1.6l/min more suitable) for after 1.6l/min purging 10min, be calculated as m1.
Purge flow rate choice experiment table
5. computing formula is:
Slurry solid content is pressed formula (1) and is calculated:
In formula:
C: slurry solid content, is represented with mass fraction, %；
m1: the quality after samples dried, unit is gram (g)；
m0: sample mass, unit is gram (g).
Arbitrary technical scheme disclosed in the invention described above unless otherwise stated, if it discloses numerical range, then
Disclosed numerical range is preferred numerical range, any it should be appreciated by those skilled in the art: preferably numerical range
It is only the obvious or representative numerical value of technique effect in many enforceable numerical value.Due to numerical value more it is impossible to
Exhaustion, so the present invention just discloses component values to illustrate technical scheme, and, the above-mentioned numerical value enumerated is not
The restriction to the invention protection domain should be constituted.
Finally it should be noted that: above example is only not intended to limit in order to technical scheme to be described；To the greatest extent
Pipe has been described in detail to the present invention with reference to preferred embodiment, and those of ordinary skill in the art are it is understood that still
The specific embodiment of the present invention can be modified or equivalent is carried out to some technical characteristics；Without deviating from this
The spirit of bright technical scheme, it all should be covered in the middle of the technical scheme scope that the present invention is claimed.
Claims (4)
1. a kind of detection method of slurry solid content it is characterised in that: comprise the following steps:
A. take a certain amount of chlorosilane slurry sample and weigh；
B. the chlorosilane slurry sample through stirring carries out centrifugal treating with centrifuge；
C. it is passed through nitrogen and purge out remaining volatile chlorosilane liquid produced；
D. weigh up the quality of remaining solid, draw the solid content in slurry.
2. a kind of slurry solid content according to claim 1 detection method it is characterised in that: by agitated chlorosilane
Slurry sample is placed in the centrifuge tube being pre-dried and weighing, and places into and carries out centrifugal treating in centrifuge.
3. a kind of slurry solid content according to claim 1 detection method it is characterised in that: by effusion meter connect from
Heart test tube and nitrogen pipeline, then carry out nitrogen purging.
4. a kind of slurry solid content according to claim 2 detection method it is characterised in that: described centrifuge tube be resistance to
Corrosion material is made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611004758.8A CN106370553A (en) | 2016-11-15 | 2016-11-15 | Method for detecting solid content of slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611004758.8A CN106370553A (en) | 2016-11-15 | 2016-11-15 | Method for detecting solid content of slurry |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106370553A true CN106370553A (en) | 2017-02-01 |
Family
ID=57894529
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611004758.8A Pending CN106370553A (en) | 2016-11-15 | 2016-11-15 | Method for detecting solid content of slurry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106370553A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110018114A (en) * | 2019-04-12 | 2019-07-16 | 贵州开磷集团矿肥有限责任公司 | A method of solid content of phosphoric acid is quickly measured using centrifuge |
| CN110208138A (en) * | 2019-06-10 | 2019-09-06 | 甘肃路桥建设集团有限公司 | A kind of accelerator solid content intellectualized detection method |
| CN112083122A (en) * | 2019-06-15 | 2020-12-15 | 北京建筑材料科学研究总院有限公司 | Method for rapidly detecting content of insoluble substances in garbage fly ash washing slurry |
| CN112824869A (en) * | 2019-11-20 | 2021-05-21 | 新疆建筑科学研究院（有限责任公司） | Method for detecting solid content of waste slurry and waste liquid |
| CN113447395A (en) * | 2021-08-10 | 2021-09-28 | 湖北中烟工业有限责任公司 | Detection device for detecting slag content of coating liquid for papermaking-method tobacco sheets |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203909003U (en) * | 2014-06-12 | 2014-10-29 | 陕西天宏硅材料有限责任公司 | Online detection sample handling device for liquid-state chlorosilane |
| CN204214707U (en) * | 2014-11-11 | 2015-03-18 | 亚洲硅业（青海）有限公司 | A kind of pretreating device for analyzing trace impurity in trichlorosilane |
| CN105377392A (en) * | 2013-04-09 | 2016-03-02 | 瓦克化学股份公司 | Apparatus and process for treating liquids containg chlorosilanes |
| CN105547905A (en) * | 2015-12-28 | 2016-05-04 | 中建商品混凝土有限公司 | Determination device and method of solid content of waste slurry of concrete mixing station |
-
2016
- 2016-11-15 CN CN201611004758.8A patent/CN106370553A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105377392A (en) * | 2013-04-09 | 2016-03-02 | 瓦克化学股份公司 | Apparatus and process for treating liquids containg chlorosilanes |
| CN203909003U (en) * | 2014-06-12 | 2014-10-29 | 陕西天宏硅材料有限责任公司 | Online detection sample handling device for liquid-state chlorosilane |
| CN204214707U (en) * | 2014-11-11 | 2015-03-18 | 亚洲硅业（青海）有限公司 | A kind of pretreating device for analyzing trace impurity in trichlorosilane |
| CN105547905A (en) * | 2015-12-28 | 2016-05-04 | 中建商品混凝土有限公司 | Determination device and method of solid content of waste slurry of concrete mixing station |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110018114A (en) * | 2019-04-12 | 2019-07-16 | 贵州开磷集团矿肥有限责任公司 | A method of solid content of phosphoric acid is quickly measured using centrifuge |
| CN110018114B (en) * | 2019-04-12 | 2022-03-11 | 贵州开磷集团矿肥有限责任公司 | Method for rapidly determining solid content of phosphoric acid by using centrifugal machine |
| CN110208138A (en) * | 2019-06-10 | 2019-09-06 | 甘肃路桥建设集团有限公司 | A kind of accelerator solid content intellectualized detection method |
| CN112083122A (en) * | 2019-06-15 | 2020-12-15 | 北京建筑材料科学研究总院有限公司 | Method for rapidly detecting content of insoluble substances in garbage fly ash washing slurry |
| CN112824869A (en) * | 2019-11-20 | 2021-05-21 | 新疆建筑科学研究院（有限责任公司） | Method for detecting solid content of waste slurry and waste liquid |
| CN113447395A (en) * | 2021-08-10 | 2021-09-28 | 湖北中烟工业有限责任公司 | Detection device for detecting slag content of coating liquid for papermaking-method tobacco sheets |
| CN113447395B (en) * | 2021-08-10 | 2022-04-12 | 湖北中烟工业有限责任公司 | Solid-liquid separation device for detecting slag content of tobacco sheet coating liquid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106370553A (en) | Method for detecting solid content of slurry | |
| Hameed | Removal of cationic dye from aqueous solution using jackfruit peel as non-conventional low-cost adsorbent | |
| Amuda et al. | Adsorption of methylene blue from aqueous solution using steam-activated carbon produced from Lantana camara stem | |
| Hasani et al. | Equilibrium and kinetic studies of azo dye (Basic Red 18) adsorption onto montmorillonite: Numerical simulation and laboratory experiments | |
| CN118184848A (en) | Control method and system for polymer purification | |
| CN105665734A (en) | Preparation method for gold-loaded tin oxide nanometer material for detecting hydrogen | |
| CN103900853B (en) | A kind of on-line period system and method for aromatization process | |
| Karandikar et al. | Effect of water on the solubilities and mass transfer coefficients of gases in a heavy fraction of fischer‐tropsch products | |
| Ding et al. | Hydrodynamic Behavior and Residence Time Distribution of Industrial‐Scale Bale Packings | |
| Higgins et al. | Dewatering characteristics of cambi thermal hydrolysis biosolids: centrifuges vs. BFPs | |
| McKay et al. | Multicomponent dye adsorption onto carbon using a solid diffusion mass-transfer model | |
| Riegel et al. | Kinetics of uranium sorption onto weakly basic anion exchangers | |
| Min et al. | A functionalized cellulose regenerative microcolumn combined with ultraviolet spectrophotometry for economic detection of selenium in purple potato | |
| Haimi et al. | Infinite dilution activity coefficient measurements by inert gas stripping method | |
| CN110433507B (en) | Method for automatically discharging silane slurry slag according to solid content | |
| CN211190621U (en) | Intelligent spiral shell centrifuge lectotype experiment circulating device that crouches | |
| CN112174996B (en) | Method and device for continuously producing silane coupling agent | |
| CN106680133A (en) | Carbon dioxide absorbent and determination method of carbon dioxide content | |
| CN113281213A (en) | Vanadium removal efficiency detection method and device | |
| CN208239374U (en) | Circulation is without gradient reaction experiment system in normal pressure | |
| CN204509208U (en) | A kind of oil-sand medium pitch thermokalite water of improvement is separated analogue experiment installation | |
| Poós et al. | Thermal dewatering of waste sludge in an agitated drum dryer | |
| CN206986075U (en) | The synthesizer of isobutyl triethoxy silane | |
| CN106498424A (en) | A kind of online recycling for spent acid utilizes system | |
| Li et al. | Statistical assessment of gas/liquid mass transfer in slurry‐phase propylene polymerization process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170201 |
|
| RJ01 | Rejection of invention patent application after publication |