CN201251573Y - Detector of alpha cellulose in pulp based on indirect method - Google Patents

Detector of alpha cellulose in pulp based on indirect method Download PDF

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Publication number
CN201251573Y
CN201251573Y CNU200820063589XU CN200820063589U CN201251573Y CN 201251573 Y CN201251573 Y CN 201251573Y CN U200820063589X U CNU200820063589X U CN U200820063589XU CN 200820063589 U CN200820063589 U CN 200820063589U CN 201251573 Y CN201251573 Y CN 201251573Y
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China
Prior art keywords
automatic
reagent
mixing arrangement
sample
control system
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Expired - Fee Related
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CNU200820063589XU
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Chinese (zh)
Inventor
黄�俊
于彬
李莉
蒲运龙
王小玲
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Yibin Grace Group Co Ltd
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YIBIN CHANGYI POMACE CO Ltd
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Abstract

The utility model discloses an automatic detecting method for alpha cellulose in pulp and a detector thereof, which aim to solve the problems of high error and long analysis time of the artificial indirect method for detecting alpha cellulose in pulp. The automatic detector of alpha cellulose in pulp based on indirect method comprises a weighing system, a sample processing system, an automatic control system and an automatic potentiometric titration control system, wherein the weighing system is composed of a weighing tray, a quality sensor and a quality monitor, the sample processing system comprises a reagent system, a mixing device and a filtrate processing system, the automatic control system is composed of a data transmission processing system and a quantitative reagent adding system, and the automatic potentiometric titration control system comprises a reagent system and an automatic titration system. Analysis errors caused by individual reasons can be reduced and analysis time can be shortened by utilizing the utility model.

Description

Pulp methyl fiber detector based on indirect method
Technical field
The utility model relates to the pulp methyl fiber detection technique, adopts indirectly specifically pulp methyl fiber is carried out the detector that robotization detects.
Background technology
Detecting pulp methyl fiber at present mainly is to adopt manual analysis.Comprise indirect method and direct method, indirect method claims volumetric method again, the direct method method that weighs again.Indirect method detects principle: each component of non-cellulose in the working sample, gained sum as a result deduct from 100 and are content of cellulose, testing process: claim partly fibre-calculating in separation (mercerization the processings)-filtration-mensuration filtrate of sample-fiber; Direct method detects principle: utilize chemical reagent (17.5% NaOH) to handle sample, make non-cellulose stripping wherein and obtain alpha-cellulose, testing process: claim the separation (mercerization processing) of sample-fiber-wash sample-oven dry-weighing-calculating.
May be when gravimetric method is analyzed because of washing in the clean and mercerization processing procedure because of there is big artificial error in individual reason, existing sample constant weight drying mode time length and influence production control; When volumetric method is analyzed during because of endpoint because of there is big artificial error in individual reason, also exist than mistake, as spectrophotometric method because of analytical approach self.For further dwindling personal error and detection time, the fine testing process of first is carried out very necessity of robotization, instrumentation mensuration.
The utility model content
The utility model is intended to detect the problem that personal error is big, analysis time is long in the method for pulp methyl fiber at existing artificial indirect method, a kind of robotization pulp methyl fiber detector based on indirect method is proposed, with the analytical error that reduces to cause and shorten analysis time owing to individual reason.
For solving the problems of the technologies described above, the technical solution adopted in the utility model is as follows:
Based on the pulp methyl fiber detector of indirect method, comprise following four parts:
Weighing system: be made up of large face plate, mass sensor, quality instrument, mass sensor is connected with large face plate, and is electrically connected with computing machine through the quality instrument, quality signal is sent to the quality instrument changes into electric signal and import computing machine again into;
Sample processing system: be made up of reagent system, mixing arrangement and filtrate disposal system, reagent system is communicated with mixing arrangement, and mixing arrangement is connected with the filtrate disposal system, and mixing arrangement comprises container and the peristaltic pump that the sample and the classes of agents of adding are mixed;
Automatic control system: by data transmission processing system, quantitatively add reagent system and form, quantitatively add reagent system and comprise the program control miniature volume pump of computer control, valve; Automatic control system is calculated the alkali lye amount of adding automatically according to sample weighting amount, and controls the automatic gauge adding of addition and other reagent automatically;
Automatic potentiometric titration control system: form by reagent system (with identical in the sample processing system), automatic titration system, current potential changes with oxidation state in the solution and the ratio of going back ortho states in the titration, when the current potential indication is reached home, computing machine to control system, stops titration with signal feedback automatically.
The beneficial effects of the utility model show:
One, reduce the analytical error that causes owing to individual reason: since the reading after terminal colour, titration everyone exist difference, thereby produce analytical error or analysis result not parallel.Adopt instrumental analysis then can reduce the analytical error that causes owing to individual reason, instrument error then can be controlled by revising.
Two, shorten analysis time: existing sample drying mode just can reach constant weight for up to 2~3 hours, and partly the fibre time can not surpass half an hour in the titration filtrate.
Description of drawings
Fig. 1 is the utility model detector structure principle chart
Embodiment
The utility model has proposed the detection method and the detector of robotization at existing manual analysis method.
One, detection method
1, about shortening detection time
Analyze the definition of fine testing process of first and first fibre, the mercerization processing procedure and the mercerization processing time of sample can't be compressed.When direct method detected the first fibre, the shortening time should consider that oven drying is adopted in existing oven dry from drying course, and the constant weight time needs more than 2 hours.If the employing micro-wave vacuum then can shorten drying time (needing about 30 minutes approximately) significantly.
The micro-wave drying processing procedure is exactly by microwave and material direct interaction, and portion is converted into very-high frequency electromagnetic energy the process of heat energy within it.Under the effect of microwave electromagnetic field, the polar molecule in the medium transfers the alternation of following microwave electromagnetic field to and oriented from original thermal motion state, in this microprocess, and the fierce friction of intermolecular generation, microwave energy is converted into the heat in the medium.And water is polar molecule, is to absorb the good medium of microwave.Traditional heat solid material must be in the environment of a heating, then from outward appearance to inner essence, is conducted into solid interior gradually, need for a long time, and microwave is to infiltrate interior of articles with the light velocity that the time is very short.Drying means such as traditional infrared, hot blast heat inhomogeneously, and energy consumption is big, and drying time is long, and microwave heating time is short, homogeneous heating, and no thermal inertia is easy to control, and the microwave penetration ability reaches 80mm.If then further shortened drying time in microwave and vacuum combination.
2, testing process
Detection method is: A, adopt potassium dichromate to make organism in the filtrate sample (that is: dissolved β, gamma cellulose) be oxidized to carbon dioxide; B, measure after the oxidation excessive potassium dichromate in the sample filtrate then.Adopt microwave that filtrate sample is heated to quicken half fine oxidizing process before the said method A step.In the said method B step, adopt the potassium dichromate oxidation reductometry, adopt, and be terminal point to being purple with the l ferrous ammonium sulfate solution titration of demarcation newly with the agent of giving instruction of ferrous Ling-Fei Luo quinoline.In the said method B step, adopt and stop the method automatic potentiometric titration forever, select Fe for use 3+/ Fe 2+Electrodes selective is determined titration end-point.
When adopting the utility model to use indirect method to detect, mainly utilize the oxidation of potassium dichromate to make the organism in the filtrate all be oxidized to carbon dioxide.Measure potassium dichromate excessive in the oxidation rear filtrate then.
Concrete assay method has (1) potassium dichromate oxidation reductometry, adopts indicator to determine titration end-point, but because terminal colour is darker, endpoint is difficult, excessive easily during titration.As select Fe for use 3+/ Fe 2+Electrodes selective adopts and stops method potentiometric titration (current potential is 0.8mv when titration end-point) (list of references " analytical chemistry ", " instrumental analysis ") forever, then can accurately judge terminal point and can realize automatic control.(2) spectrophotometric method (721 type spectrophotometer): adopting wavelength is 620nm (list of references: hemicellulose level cuts into a mountain and collects eastern Yu of chemical fibre mill's gold in the colorimetric method for determining pulp), according to the size of optical density, can record and starch the hemicellulose level that dissolves.The utility model also can adopt red, orange, green, blue, yellow (ROGBY) that organism in the filtrate is analyzed.
When measuring, need do the effect correction of different alkali charges to the fine analysis result of first with indirect method.Half fiber detecting device can adopt automatic control of Electric potentials titration, also can adopt spectrophotometric method to measure automatically.
Two, robotization detector
When design, can be divided into following several module and carry out, make up according to different schemes then:
1 Weighing system
2 sample preparation (mercerization processing) system
3 chemical reagent and distilled water add control system
4 micro-wave vacuum systems
5 automatic potentiometric titration control system
6 data transmission processing systems
Weighing system: be made up of large face plate, mass sensor, quality instrument, mass sensor is sent to the quality instrument with quality signal and changes into electric signal and import computing machine again into and handle;
Sample processing system: be made up of reagent system, mixing arrangement and filtrate disposal system, mixing arrangement comprises peristaltic pump, container; After sample and classes of agents automatically added, peristaltic pump fully mixed reagent with sample and leaves standstill mercerization then, after finishing sample is separated with classes of agents;
Automatic control system: by data transmission processing system, quantitatively add reagent system and form, quantitatively add reagent system and comprise the program control miniature volume pump of computer control, valve; Automatic control system is calculated the alkali lye amount of adding automatically according to sample weighting amount, and controls the automatic gauge adding of addition and other reagent automatically;
Automatic potentiometric titration control system: form by reagent system (with identical in the sample processing system), automatic titration system, in the titration process, oxidation state changes with the ratio of going back ortho states in the solution, current potential changes thereupon, when the current potential indication is reached home, computing machine to control system, stops titration with signal feedback automatically.
Step is as follows: drop into sample, Weighing system weighs up its quality and imports data into data transmission processing system, computer is handled data, calculate the required alkali lye consumption of the photochemical processing of sample filaments (calculating) by 2 gram sample 30ml alkali lye amounts, then information feedback is arrived automatic control system, be metered into alkali lye by miniature volume pump and carry out the mercerization processing.The mercerization processing finishes the back filters, and automatic ration (can control container by overflow achieves the goal) pipettes filtrate mensuration, and titration is adopted and stopped the method automatic potentiometric titration forever.Data after the titration are imported data transmission processing system processing and output result into.
Then can calculate the potassium dichromate amount that oxidation stripping hemicellulose is consumed after measuring excessive potassium dichromate.Rule of thumb data 1mol potassium dichromate can be calculated the fine content of first by following formula by oxidation 0.00675g half fibre:
The fine %=[1-CV*0.00675/G of first] * 100%
The concentration of c-potassium dichromate in the formula, mol/l
The volume of the potassium dichromate that v-consumes, ml
The example weight that G-takes by weighing, g
Equipment work process and principle:
Weighing system weighs up its sample quality and imports data into automatic control system, computer is handled data, calculate the required alkali lye consumption of the photochemical processing of sample filaments, be metered into alkali lye or quantitatively add (end product is proofreaied and correct by coefficient) by miniature volume pump then, under programmed control, start peristaltic pump and automatically alkali lye and the abundant mixing of sample are carried out the mercerization processing by overflow control container.The mercerization processing finishes the back and filters, automatic ration (can control container by overflow achieves the goal) pipettes filtrate to the filtrate disposal system, automatic ration (can control container by overflow achieves the goal) adds potassium dichromate again under programmed control, sulfuric acid oxidation half fibre quantitatively adds phosphoric acid and distilled water then, automatic ration (achieving the goal by overflow control container) pipettes solution again under automatic control system, with iron ammonium sulfate filtrate is measured again, titration is adopted and is stopped the method automatic potentiometric titration forever (in titration process, oxidation state changes with the ratio of going back ortho states in the solution, current potential changes thereupon), timely with the magnetic stirrer agitating solution in titration process to react fully, when the current potential indication is reached home, computing machine to control system, stops signal feedback titration and imports endpoint data into data transmission processing system handling and export the result automatically.The operating control signal of pump and valve, time control signal etc. are controlled by automatic control system in the system.
Wherein individual component is not further elaborated, and is because be the routine techniques that those of ordinary skills know, and such as the filtrate disposal system, promptly according to the utility model thought filtrate is handled.

Claims (1)

1,, comprise following four parts based on the pulp methyl fiber detector of indirect method:
Weighing system: be made up of large face plate, mass sensor, quality instrument, mass sensor is connected with large face plate, and is electrically connected with computing machine through the quality instrument, quality signal is sent to the quality instrument changes into electric signal and import computing machine again into;
Sample processing system: be made up of reagent system, mixing arrangement and filtrate disposal system, reagent system is communicated with mixing arrangement, and mixing arrangement is connected with the filtrate disposal system, and mixing arrangement comprises container and the peristaltic pump that the sample and the classes of agents of adding are mixed;
Automatic control system: by data transmission processing system, quantitatively add reagent system and form, quantitatively add reagent system and comprise the program control miniature volume pump of computer control, valve, be located between reagent system and the mixing arrangement, and be electrically connected with computing machine;
Automatic potentiometric titration control system: be connected with computing machine, pressure regulator, time controller respectively, and machine is controlled program control miniature volume pump as calculated, valve is communicated with ferrous sulphate ammonium reagent in the reagent system.
CNU200820063589XU 2008-05-30 2008-05-30 Detector of alpha cellulose in pulp based on indirect method Expired - Fee Related CN201251573Y (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101281188B (en) * 2008-05-30 2011-07-20 宜宾长毅浆粕有限责任公司 Method for detecting dissolving pulp methyl fiber based on indirect method
CN102645361A (en) * 2012-04-24 2012-08-22 柳州职业技术学院 Automatic treatment device for animal feed AFB1 content detection sample
CN106996919A (en) * 2016-01-25 2017-08-01 西派特(北京)科技有限公司 A kind of instrument for detecting a variety of properties of slurry pool
CN108020483A (en) * 2018-01-25 2018-05-11 杭州神农牧业有限公司 Neutral detergent fiber measurement device

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101281188B (en) * 2008-05-30 2011-07-20 宜宾长毅浆粕有限责任公司 Method for detecting dissolving pulp methyl fiber based on indirect method
CN102645361A (en) * 2012-04-24 2012-08-22 柳州职业技术学院 Automatic treatment device for animal feed AFB1 content detection sample
CN102645361B (en) * 2012-04-24 2013-11-06 柳州职业技术学院 Automatic treatment device for animal feed AFB1 content detection sample
CN106996919A (en) * 2016-01-25 2017-08-01 西派特(北京)科技有限公司 A kind of instrument for detecting a variety of properties of slurry pool
CN108020483A (en) * 2018-01-25 2018-05-11 杭州神农牧业有限公司 Neutral detergent fiber measurement device

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Owner name: YIBIN GRACE GROUP COMPANY

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Effective date: 20130520

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Effective date of registration: 20130520

Address after: 644002 space Road, Nan'an economic and Technological Development Zone, Yibin, Sichuan

Patentee after: Yibin Grace Group Company

Address before: 644002 Yibin, South Bank of the middle of the road, the space shuttle

Patentee before: Yibin Changyi Pomace Co., Ltd.

CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20090603

Termination date: 20150530

EXPY Termination of patent right or utility model