CN109731846A - Full-automatic elution instrument and its application method - Google Patents

Full-automatic elution instrument and its application method Download PDF

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Publication number
CN109731846A
CN109731846A CN201910112185.8A CN201910112185A CN109731846A CN 109731846 A CN109731846 A CN 109731846A CN 201910112185 A CN201910112185 A CN 201910112185A CN 109731846 A CN109731846 A CN 109731846A
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China
Prior art keywords
elution
eluent
container
control valve
waste liquid
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CN201910112185.8A
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CN109731846B (en
Inventor
徐英杰
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China Titanium Group Jiaozuo Yusheng Titanium Industry Co Ltd
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China Titanium Group Jiaozuo Yusheng Titanium Industry Co Ltd
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Abstract

The invention belongs to the production technical fields of high-purity raw, Impurity elution full-automatic elution instrument and its application method in a kind of raw material are provided, including filtrate analysis device, filtrate delivery pump, eluent delivery pump, acidity-basicity sensor, eluant, eluent control valve, eluent stream scale, clean hydraulic control valve, wash liquid stream scale, waste liquid control valve, waste liquid flowmeter, blender is equal, console etc., its application method includes that will elute raw material to launch into elution container, eluant, eluent is launched into elution container, open filtrate delivery pump, filtrate is transported to analytical equipment;Waste liquid control valve is opened, waste liquid is discharged;The cleaning agent in detergent container is allowed to launch into elution container, judge whether pH value reaches clean endpoint standard, throwing raw materials of the present invention, after the conditions such as input elution, cleaning, remaining whole process realizes full automatic working, the real-time detection of impurity concentration and pH value is realized, realizes the minimum of elution, cleaning agents useful for same.

Description

Full-automatic elution instrument and its application method
Technical field
The invention belongs to the production technical field of high-purity raw, a kind of full-automatic elution instrument and its application method are provided.
Background technique
Titanium dioxide (being commonly called as titanium dioxide) is that one kind is widely used in the fields such as paint, plastics, pharmacy, food, cosmetics White pigment ingredient.Due in raw mineral materials impurity or extractive process in the reason of reagent added, the works such as paint, plastics It is not usually able to satisfy food, medicine containing the objectionable impurities such as various micro heavy metals (such as: lead and arsenic) in industry grade titanium dioxide The relevant criterion (non-patent literature 1, non-patent literature 2, non-patent literature 3) of product, cosmetics.
In order to reduce the objectionable impurities content such as heavy metal in industrial grade titanium dioxide, patent document 1 and patent document 2 divide Not providing can selecting technology.But specific device is not provided in these documents.
Due to needing to use the hazardous agents being harmful to the human body in elution process, such as various organic acids and inorganic acid, manpower There is very big risk to the health hazard of operator when operation.
In addition, due to manual operation it is stringent since in the technical level of operator, be easy to cause on end product quality Fluctuation.
In order to avoid, to the health hazard of operator, and realizing stable quality management in production process, the present invention is mentioned For a kind of automatic washing desorption method.
3. pertinent literature:
Non-patent literature 1:GB25577-2010, " national food safety standard: food additives titanium dioxide ".
Non-patent literature 2: " Chinese Pharmacopoeia " (2015 editions), state food pharmaceuticals administration general bureau (CFDA).
Non-patent literature 3:GB-27599-2011, " National Standard of the People's Republic of China: titanium dioxide used for cosmetic ".
Patent document 1:CN105110365A, " a kind of production system and its production technology of food-level titanium dioxide ".
Patent document 2:CN101920992B, " preparation method of food-level titanium dioxide ".
Based on above-mentioned prior art, the applicant has made lasting and beneficial exploration and design repeatedly, and carries out The test of non-finite number of time has finally found the method for solving above-mentioned technical problem and forms technology described below Scheme.
Summary of the invention
To solve problem of the prior art, the present invention provides a kind of full-automatic elution instrument of Impurity elution in raw material and its Application method.
In order to achieve the above object, the invention adopts the following technical scheme: a kind of full-automatic elution instrument, including blender, The blender top is provided with elution container, and stirrer is equipped in elution container, and blender drive stirrer, which is realized, to be held The mixing of raw material and eluant, eluent and cleaning solution in device, elution are equipped with elution raw material layer with container is interior, and elution is set with container side There is liquid waste filter, liquid waste filter is connect with waste liquid control valve, and waste liquid control valve is connect with waste liquid flowmeter, waste liquid flowmeter It is set to waste liquid pool side, elution is connected with container with soda liquor container, and soda liquor container is connect with cleaning hydraulic control valve, clearly Washing lotion control valve is connect with wash liquid stream scale, and wash liquid stream scale is connected by wash liquid stream buret and elution with container, is washed De- to be connect with container with elution agent container, elution agent container is connect with eluant, eluent control valve, eluant, eluent control valve and eluent stream Scale connection, eluent stream scale are connected by eluent stream buret and elution with container, and acidity-basicity sensor end is set to In elution raw material layer in elution container, eluent delivery pump is connect with eluent delivery pipe, and eluent delivery pipe is set to It elutes in raw material layer, eluent delivery pump is connect with pot strainer, and pot strainer is connect with filtrate delivery pump, filtrate conveying Pump is connect with filtrate analysis device, and filtrate analysis device is connect with pot strainer, and pot strainer passes through screen pipe and elution It is connected with container, filtrate analysis device, eluent delivery pump, acidity-basicity sensor, eluant, eluent control valve, is washed filtrate delivery pump De- agent flux table, cleaning hydraulic control valve, wash liquid stream scale, waste liquid control valve, waste liquid flowmeter and blender are and console Pass through connection.
A kind of application method of full-automatic elution instrument, includes the following steps:
1) elution raw material is launched into elution container, the amount of the raw material of dispensing is input to console;
2) setting elution and cleaning index;
3) eluant, eluent control valve is opened, the eluant, eluent in elution agent container is allowed to launch into elution container;
4) numerical value of eluent stream scale is observed;
5) after the eluant, eluent of dispensing reaches predetermined amount, eluant, eluent control valve is closed;
6) turn on agitator mixes eluant, eluent and raw material using stirrer;
7) eluent delivery pump is opened, eluent is transported to pot strainer;
8) filtrate delivery pump is opened, filtrate is transported to analytical equipment;
9) impurity concentration in analytical equipment analysis filtrate is utilized;
10) when the impurity concentration in filtrate reaches stable, no longer rises, blender and eluent delivery pump is closed and filtrate is defeated Send pump;
11) waste liquid control valve is opened, waste liquid is discharged;
12) numerical value of waste liquid flowmeter is observed;
13) after the discharging of waste liquid of discharge finishes, waste liquid control valve is closed;
14) judge whether impurity concentration reaches elution endpoint criterion, if not up to standard, repeat above-mentioned eluant, eluent and launch to useless The process of liquid discharge;If up to standard, operated into next step;
15) cleaning agent control valve is opened, the cleaning agent in detergent container is allowed to launch into elution container;
16) numerical value of cleaning agent flowmeter is observed;
17) after the cleaning agent of dispensing reaches predetermined amount, cleaning agent control valve is closed;
18) turn on agitator mixes cleaning agent and raw material using stirrer;
19) pH value that acidity-basicity sensor measures is read;
20) when pH value reaches stable, no longer changes, blender is closed;
21) waste liquid control valve is opened, waste liquid is discharged;
22) numerical value of waste liquid flowmeter is observed;
23) after the discharging of waste liquid of discharge finishes, waste liquid control valve is closed;
24) judge whether pH value reaches clean endpoint standard, if not up to standard, repeat above-mentioned cleaning agent and launch to waste liquid The process of discharge;If up to standard, operated into next step;
25) entire elution, cleaning process terminate.
Blender selects the mode of magnetic stirring apparatus or ultrasonic activation to carry out raw material and eluant, eluent, clear in the step 6) The mixing of lotion.
Compared with prior art, advantageous effect of the invention is:
1. throwing raw materials input after the conditions such as elution, cleaning, remaining whole process realizes full automatic workings.
2. whole flow process, realizes the real-time detection of impurity concentration and pH value, both may be implemented used in elution, cleaning The minimum of reagent, and may insure that the quality of final products is stablized.
3. the automation of elution process avoids the intervention of operator, hazardous agents is prevented and operator have been good for Health harm.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention, Objects and advantages will become more apparent upon.
Fig. 1: the structure chart of the full-automatic elution process of the present invention
Fig. 2: the operating process of the full-automatic elution process of the present invention.
Specific embodiment
The present invention is described in further details below by embodiment, embodiment is only used to illustrate the present invention, and unlimited The scope of the present invention processed.
A kind of full-automatic elution instrument as shown in Figs. 1-2 and its application method, including blender 4, the setting of 4 top of blender There is elution container 1, stirrer 3 is equipped in elution container 1, blender 4 drives stirrer 3 to realize raw material and elution in container Agent and the mixing of cleaning solution, elution are equipped with elution raw material layer 2 with container 1 is interior, and elution is with 1 side of container equipped with liquid waste filter 13, liquid waste filter 13 is connect with waste liquid control valve 14, and waste liquid control valve 14 is connect with waste liquid flowmeter 15, waste liquid flowmeter 15 It is set to 16 side of waste liquid pool, elution container 1 is connected with soda liquor container 17, soda liquor container 17 and cleaning hydraulic control valve 18 connection, cleaning hydraulic control valve 18 connect with wash liquid stream scale 19, wash liquid stream scale 19 pass through wash liquid stream buret 191 and Elution is connected with container 1, and elution is connect with container 1 with elution agent container 5, and elution agent container 5 is connect with eluant, eluent control valve 6, Eluant, eluent control valve 6 is connect with eluent stream scale 7, and eluent stream scale 7 passes through eluent stream buret 71 and elution container 1 Connection, 20 end of acidity-basicity sensor are set in the elution raw material layer 2 in elution container 1, eluent delivery pump 8 and elution Liquid delivery pipe 81 connects, and eluent delivery pipe 81 is set in elution raw material layer 2, and eluent delivery pump 8 and pot strainer 9 connect It connects, pot strainer 9 is connect with filtrate delivery pump 10, and filtrate delivery pump 10 is connect with filtrate analysis device 11, filtrate analysis dress It sets 11 to connect with pot strainer 9, pot strainer 9 is connect with elution with container 1 by screen pipe 91, filtrate analysis device 11, filtrate delivery pump 10, eluent delivery pump 8, acidity-basicity sensor 20, eluant, eluent control valve 6, eluent stream scale 7, cleaning Hydraulic control valve 18, wash liquid stream scale 19, waste liquid control valve 14, waste liquid flowmeter 15 and blender 4 pass through with console 12 Connection.12 producer of console selects National Instruments, model: NI USB-6289,9 factory of pot strainer Family selects Sai Duolisi, model: Vivaflow 200, and 11 producer of filtrate analysis device selects: Agilent, model: Agilent7800, or select producer Micro Emission, model: MH-6000A.
The application method of the full-automatic elution instrument, includes the following steps:
Elution raw material 2 is launched to elution in container 1, the amount of the raw material of dispensing is input to console 12;
Setting elution and cleaning index: the proportion including eluant, eluent and raw material;Elute discrimination standard (such as the impurity lead of terminal Concentration);The proportion of cleaning solution and raw material;The judgment criteria (such as pH value is between pH 6.0 to pH 8.0) of clean endpoint;
Eluant, eluent control valve 6 is opened, the eluant, eluent in elution agent container 5 is allowed to launch into elution container 1;
Observe the numerical value of eluent stream scale 7;
After the eluant, eluent of dispensing reaches predetermined amount, eluant, eluent control valve 6 is closed;(injected volume can according to the amount of raw material, wash The proportion of de- agent and raw material, the numerical value of eluent stream scale and release time calculate)
Turn on agitator 4 mixes eluant, eluent and raw material using stirrer 3;
Eluent delivery pump 8 is opened, eluent is transported to pot strainer 9;
Filtrate delivery pump 10 is opened, filtrate is transported to analytical equipment 11;
The impurity concentration in filtrate is analyzed using analytical equipment 11;
When the impurity concentration in filtrate reaches stable, no longer rises, blender 4, eluent delivery pump 8 and filtrate conveying are closed Pump 10;
Waste liquid control valve 14 is opened, waste liquid is discharged;
Observe the numerical value of waste liquid flowmeter 15;
After the discharging of waste liquid of discharge finishes, waste liquid control valve 15 is closed;
Judge whether impurity concentration reaches elution endpoint criterion, if not up to standard, repeat above-mentioned eluant, eluent and launch to waste liquid The process of discharge;If up to standard, operated into next step;
Cleaning agent control valve 18 is opened, the cleaning agent in detergent container 17 is allowed to launch into elution container 1;
Observe the numerical value of cleaning agent flowmeter 19;
After the cleaning agent of dispensing reaches predetermined amount, cleaning agent control valve 18 is closed;(injected volume can according to the amount of raw material, The proportion of cleaning agent and raw material, the numerical value of cleaning agent flowmeter and release time calculate)
Turn on agitator 4 mixes cleaning agent and raw material using stirrer 3;
Read the pH value that acidity-basicity sensor 20 measures;
When pH value reaches stable, no longer changes, blender 4 is closed;
Waste liquid control valve 14 is opened, waste liquid is discharged;
Observe the numerical value of waste liquid flowmeter 15;
After the discharging of waste liquid of discharge finishes, waste liquid control valve 15 is closed;
Judge whether pH value reaches clean endpoint standard, if not up to standard, repeat above-mentioned cleaning agent and launch to waste liquid row The process put;If up to standard, operated into next step;
Entire elution, cleaning process terminate.The fully automatic add of eluant, eluent, cleaning agent in the present invention automatically controls;Eluent On-line filtration and real-time impurity concentration test;The combination of addition, the control of the real-time monitoring and eluant, eluent of impurity concentration is realized Elution terminal judges automatically;Addition, the control of pH value real-time monitoring and cleaning agent combine, and realize the automatic of clean endpoint Judgement.
Blender selects the mode of magnetic stirring apparatus or ultrasonic activation to carry out raw material and eluant, eluent, clear in the step 6) The mixing of lotion.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc. Imitate embodiment.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to above embodiments institute Any simple modification, equivalent variations and the remodeling made, still fall within the protection scope of technical solution of the present invention.

Claims (3)

1. a kind of full-automatic elution instrument, including blender, it is characterised in that: the blender top is provided with elution container, Stirrer is equipped in elution container, blender drive stirrer realizes the mixing of raw material and eluant, eluent and cleaning solution in container, Elution raw material layer is equipped in elution container, elution container side is equipped with liquid waste filter, and liquid waste filter and waste liquid control Valve connection, waste liquid control valve are connect with waste liquid flowmeter, and waste liquid flowmeter is set to waste liquid pool side, elution container and cleaning Liquid container is connected, and soda liquor container is connect with cleaning hydraulic control valve, and cleaning hydraulic control valve is connect with wash liquid stream scale, cleans Liquid stream scale is connected by wash liquid stream buret and elution with container, and elution is connect with container with elution agent container, and eluant, eluent holds Device is connect with eluant, eluent control valve, and eluant, eluent control valve is connect with eluent stream scale, and eluent stream scale passes through eluent stream Buret and elution are connected with container, and acidity-basicity sensor end is set in the elution raw material layer in elution container, eluent Delivery pump is connect with eluent delivery pipe, and eluent delivery pipe is set in elution raw material layer, eluent delivery pump and online mistake Filter connection, pot strainer are connect with filtrate delivery pump, and filtrate delivery pump is connect with filtrate analysis device, filtrate analysis device It is connect with pot strainer, pot strainer is connected by screen pipe and elution with container, filtrate analysis device, filtrate conveying Pump, eluent delivery pump, acidity-basicity sensor, eluant, eluent control valve, eluent stream scale, cleaning hydraulic control valve, wash liquid stream Scale, waste liquid control valve, waste liquid flowmeter and blender pass through connection with console.
2. a kind of application method of full-automatic elution instrument according to claim 1, which comprises the steps of:
1) elution raw material is launched into elution container, the amount of the raw material of dispensing is input to console;
2) setting elution and cleaning index;
3) eluant, eluent control valve is opened, the eluant, eluent in elution agent container is allowed to launch into elution container;
4) numerical value of eluent stream scale is observed;
5) after the eluant, eluent of dispensing reaches predetermined amount, eluant, eluent control valve is closed;
6) turn on agitator mixes eluant, eluent and raw material using stirrer;
7) eluent delivery pump is opened, eluent is transported to pot strainer;
8) filtrate delivery pump is opened, filtrate is transported to analytical equipment;
9) impurity concentration in analytical equipment analysis filtrate is utilized;
10) when the impurity concentration in filtrate reaches stable, no longer rises, blender and eluent delivery pump is closed and filtrate is defeated Send pump;
11) waste liquid control valve is opened, waste liquid is discharged;
12) numerical value of waste liquid flowmeter is observed;
13) after the discharging of waste liquid of discharge finishes, waste liquid control valve is closed;
14) judge whether impurity concentration reaches elution endpoint criterion, if not up to standard, repeat above-mentioned eluant, eluent and launch to useless The process of liquid discharge;If up to standard, operated into next step;
15) cleaning agent control valve is opened, the cleaning agent in detergent container is allowed to launch into elution container;
16) numerical value of cleaning agent flowmeter is observed;
17) after the cleaning agent of dispensing reaches predetermined amount, cleaning agent control valve is closed;
18) turn on agitator mixes cleaning agent and raw material using stirrer;
19) pH value that acidity-basicity sensor measures is read;
20) when pH value reaches stable, no longer changes, blender is closed;
21) waste liquid control valve is opened, waste liquid is discharged;
22) numerical value of waste liquid flowmeter is observed;
23) after the discharging of waste liquid of discharge finishes, waste liquid control valve is closed;
24) judge whether pH value reaches clean endpoint standard, if not up to standard, repeat above-mentioned cleaning agent and launch to waste liquid The process of discharge;If up to standard, operated into next step;
25) entire elution, cleaning process terminate.
3. the application method of full-automatic elution instrument according to claim 2, it is characterised in that: blender in the step 6) The mode of magnetic stirring apparatus or ultrasonic activation is selected to carry out the mixing of raw material and eluant, eluent, cleaning agent.
CN201910112185.8A 2019-02-13 2019-02-13 Full-automatic elution instrument and use method thereof Active CN109731846B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002517753A (en) * 1998-06-08 2002-06-18 エムイーエムシー・エレクトロニック・マテリアルズ・インコーポレイテッド Method for monitoring the concentration of metal impurities in a wafer cleaning solution
CN1590303A (en) * 2003-08-28 2005-03-09 北京有色金属研究总院 Ultrasonic cleaning method of manganese dioxide
CN2876069Y (en) * 2006-02-28 2007-03-07 濮晓明 Reaction kettle use for purification treatment of quartz sand
CN102029271A (en) * 2010-11-08 2011-04-27 连云港晶族新材料科技有限公司 Quartz sand purifying and cleaning device and technique
JP2012092194A (en) * 2010-10-26 2012-05-17 Kao Corp Powder detergent composition for automatic washer
CN202984174U (en) * 2012-12-15 2013-06-12 河南富耐克超硬材料股份有限公司 Micro powder purification production device

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002517753A (en) * 1998-06-08 2002-06-18 エムイーエムシー・エレクトロニック・マテリアルズ・インコーポレイテッド Method for monitoring the concentration of metal impurities in a wafer cleaning solution
CN1590303A (en) * 2003-08-28 2005-03-09 北京有色金属研究总院 Ultrasonic cleaning method of manganese dioxide
CN2876069Y (en) * 2006-02-28 2007-03-07 濮晓明 Reaction kettle use for purification treatment of quartz sand
JP2012092194A (en) * 2010-10-26 2012-05-17 Kao Corp Powder detergent composition for automatic washer
CN102029271A (en) * 2010-11-08 2011-04-27 连云港晶族新材料科技有限公司 Quartz sand purifying and cleaning device and technique
CN202984174U (en) * 2012-12-15 2013-06-12 河南富耐克超硬材料股份有限公司 Micro powder purification production device

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