CN112557584A - Automatic titrator for terminal carboxyl content and titration method thereof - Google Patents
Automatic titrator for terminal carboxyl content and titration method thereof Download PDFInfo
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- CN112557584A CN112557584A CN202011615226.4A CN202011615226A CN112557584A CN 112557584 A CN112557584 A CN 112557584A CN 202011615226 A CN202011615226 A CN 202011615226A CN 112557584 A CN112557584 A CN 112557584A
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- 238000004448 titration Methods 0.000 title claims abstract description 40
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 title claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 45
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 42
- 238000010992 reflux Methods 0.000 claims abstract description 40
- 238000009833 condensation Methods 0.000 claims abstract description 25
- 230000005494 condensation Effects 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims description 34
- 238000003860 storage Methods 0.000 claims description 25
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- 230000000007 visual effect Effects 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims 2
- 238000009529 body temperature measurement Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 229920000728 polyester Polymers 0.000 abstract description 10
- 238000012360 testing method Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 229960001701 chloroform Drugs 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- YLLIGHVCTUPGEH-UHFFFAOYSA-M potassium;ethanol;hydroxide Chemical compound [OH-].[K+].CCO YLLIGHVCTUPGEH-UHFFFAOYSA-M 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 230000009191 jumping Effects 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/0099—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor comprising robots or similar manipulators
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
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Abstract
本发明提供一种端羧基含量自动滴定仪及其滴定方法，包括工作平台、样品杯移动机构、冷凝移动机构和试剂添加机构，工作平台包括样品区、加液滴定区、加热回流区和冷凝等待区，样品杯移动机构在工作平台内作三维运动，通过样品杯移动机构将工作平台内的样品杯移动，冷凝移动机构在工作品平台内作二维运动，冷凝移动机构将冷凝管移动与样品杯对接；试剂添加机构在加液滴定区移动，试剂添加机构对样品杯进行试剂添加；通过机械机构将样品杯在样品区、加液滴定和加热回流工位移动，通过试剂添加机构和冷凝回流机构，自动完成样品试剂添加、加热回流和滴定，不断检测溶液颜色并判定测试终点；步骤严格遵守标准要求，精确高效测定PET聚酯切片中端羧基含量。
The invention provides an automatic titrator for carboxyl end content and a titration method thereof, including a working platform, a sample cup moving mechanism, a condensation moving mechanism and a reagent adding mechanism. The working platform includes a sample area, an addition titration area, a heating reflux area and a condensation waiting area. The sample cup moving mechanism makes three-dimensional movement in the working platform, the sample cup in the working platform is moved by the sample cup moving mechanism, the condensation moving mechanism makes two-dimensional movement in the working platform, and the condensation moving mechanism moves the condensation tube to the sample. The cup is docked; the reagent adding mechanism moves in the titration area, and the reagent adding mechanism adds reagents to the sample cup; the sample cup is moved in the sample area, the titration and heating and reflux stations through the mechanical mechanism, and the reagent adding mechanism and condensation reflux The mechanism automatically completes the addition of sample reagents, heating and refluxing and titration, continuously detects the color of the solution and determines the test end point; the steps strictly follow the standard requirements, and the content of terminal carboxyl groups in PET polyester chips is accurately and efficiently determined.
Description
Technical Field
The invention relates to the technical field of terminal carboxyl content determination, in particular to an automatic titrator for terminal carboxyl content and a titration method thereof.
Background
The carboxyl end group content is a value calculated from the volume consumed by titrating a sample in a mixed solvent by using bromophenol blue as an indicator and a potassium hydroxide-ethanol standard titration solution after cooling, and expressed in millimoles per kilogram (mmol/kg). In the production process of the bottle-grade polyester chip, the content of the terminal carboxyl has very important influence on the quality of injection molding and bottle blowing in the next procedure, so that the accurate determination of the content of the terminal carboxyl in the polyester chip has very important significance for controlling the quality of a final product.
The terminal carboxyl content in the standards of GB/T17931-2018 polyethylene terephthalate (PET) resin for bottles, GB/T14190-2017 Polyester (PET) slice test method and the like is an important performance index, and the detection method for the items in the standards is defined as follows:
the sample was pulverized to a particle size of 2 mm or less (to prevent overheating of the sample at the time of pulverization). Weighing about 1.5-2 g of sample (accurate to 0.1 mg), putting the sample into a ground triangular flask, adding 50mL of phenol/trichloromethane mixed solvent, heating and refluxing until the sample is completely dissolved within 1h, and cooling to room temperature. And adding 5-6 drops of bromophenol blue indicator into the dissolved sample, titrating with a potassium hydroxide-ethanol standard titration solution (0.05 mol/L), and recording the consumption milliliter number of the standard titration solution when the solution is changed from yellow to blue, namely the titration end point. Blank test was performed under the same conditions. (for full dull slice, because of high titanium dioxide content make solution opaque milk white, the color change of the end point is difficult to judge, add 100 mL solvent or weigh 1.5 g sample, achieve the purpose of diluting titanium dioxide, convenient end point color change judge.)
The test method has the following problems in practical implementation:
1. the method is purely manually operated, and has low automation degree: the operations of liquid adding, titration, end point judgment and the like are completely implemented manually, the operation is relatively complex, the subjectivity is strong, the workload is large, and the requirement on the experience of operators is high.
2. The detection process is dangerous: the inspector needs to use solvents such as phenol, trichloromethane and the like; in the testing process, the sample needs to be heated and refluxed, then the container needs to be transferred to an operation table for the next step of test, and if the high-temperature operation fails, the scalding risk is caused, and the danger is high.
Disclosure of Invention
The invention aims to provide an automatic titrator for terminal carboxyl group content and a titration method thereof, and solves the problem that the existing terminal carboxyl group content determination is carried out by pure manual operation and the process is dangerous.
In order to achieve the purpose, the technical scheme of the invention is as follows:
an automatic titrator for terminal carboxyl content is characterized by comprising a working platform, a sample cup moving mechanism, a condensation moving mechanism and a reagent adding mechanism;
the working platform comprises a sample area, a liquid adding titration area, a heating reflux area and a condensation waiting area;
the sample cup moving mechanism moves in the left-right direction, the front-back direction and the up-down direction in the working platform, the sample cup in the working platform is moved to a specified position through the movement of the sample cup moving mechanism, and the cup opening of the sample cup is frosted;
the condensation moving mechanism moves the condensation pipe to the heating reflux area to be butted with the sample cup in the left-right and up-down directions in the working product platform;
the reagent adding mechanism moves back and forth in the liquid adding titration area and adds the specified reagent to the sample cup placed in the station.
Furthermore, a sample storage position is arranged on the sample area, sensing equipment is arranged in the sample storage position, the position of the sample is sensed through the sensing equipment, the sensing equipment sends a coordinate signal of the sample to the sample cup moving mechanism, and the sample cup moving mechanism sequentially grabs the sample according to the position of the sample.
Further, each sample area comprises at least one sample storage position, and each sample storage position is provided with a temperature measuring device.
Furthermore, at least one liquid adding drop positioning is arranged in the liquid adding titration area, a visual recognition mechanism is arranged on the liquid adding drop positioning or the reagent adding mechanism, and a homogenizing mechanism is also arranged on the liquid adding drop positioning.
Further, the visual recognition mechanism includes a light source that irradiates light to the sample and a color recognition detector that detects the color of the sample in real time or at regular time.
Furthermore, at least one heating reflux position is arranged in the heating reflux area, and a heating device, a temperature control device, a timer, a gravity sensor and a homogenizing mechanism are arranged on the heating reflux position.
Further, the sample cup moving mechanism comprises an X-axis unit, a Y1-axis unit and a Z1-axis unit which are perpendicular to each other;
the X-axis unit comprises a fixed surface, and a track is arranged on the fixed surface;
the Y1 shaft unit comprises a Y1 shaft moving arm, the Y1 shaft moving arm is installed on the X shaft fixing surface, the Y1 shaft moving arm moves along the track of the fixing surface, and the Y1 shaft moving arm is provided with a track;
the Z1 axle unit comprises a Z axle vertical moving arm which is arranged on a Y1 axle moving arm and moves along the track of the Y1 axle moving arm, and the end part of the Z1 axle vertical moving arm is provided with a clamping mechanism.
Further, the condensation moving mechanism includes an X-axis unit, a Y2-axis unit, and a Z2-axis unit, which are perpendicular to each other;
the Y2 axis unit comprises a Y2 axis moving arm, the Y2 axis moving arm is installed on the X axis fixing surface, and the Y2 axis moving arm moves along the track;
the Z2 axle unit includes an at least condenser pipe, the condenser pipe is installed on Y2 axle traveling arm, the condenser pipe moves up and down along Z2 axle unit, the lower extreme of condenser pipe is equipped with the dull polish, condenser pipe and sample cup pass through dull polish butt joint sealing.
Further, the reagent adding mechanism comprises a Y3 shaft unit, at least one adding liquid titration end and at least three reagent storage tanks;
the Y3 axle unit and the X axle unit are mutually right-angled to construct a plane parallel to the working platform, the Y3 axle unit comprises a Y3 axle fixing arm and a linear sliding table, and the Y3 axle fixing arm is arranged on the X axle fixing surface;
the straight line slip table is installed on Y3 axle fixed arm, the straight line slip table slides around the track of Y3 axle fixed arm, the end is decided to the liquid that adds is installed on the straight line slip table, the end is decided to the liquid that adds includes an at least feed liquor end and an at least play liquid end.
The invention moves the sample cup in the sample area, the liquid adding titration station, the heating reflux station and other stations through the mechanical mechanism, automatically completes the reagent adding, the heating reflux and the titration of the sample through the reagent adding mechanism and the condensation reflux mechanism, and determines the test end point through continuously detecting the color of the solution; the detection process completely conforms to the method of the national standard GB/T14190-2017 fiber-grade Polyester (PET) slice test method, the reagents and steps strictly comply with the standard requirements, and the content of terminal carboxyl groups in the PET polyester slice can be accurately and efficiently determined.
Drawings
FIG. 1 is a schematic layout of a working platform of an automatic titrator for terminal carboxyl group content according to the present invention;
reference numerals: 100a working platform; 101 a sample area; 102 liquid titration zone; 103 heating the reflux zone; 104 a condensation waiting area;
FIG. 2 is a schematic structural diagram of an automatic titrator for terminal carboxyl group content according to the present invention;
reference numerals: 201 a fixed surface; 202 track; 203 moving the arm; 204 vertically moving the arm; 205 moving the arm; 206 a condenser tube; 207 a fixed arm; 208 linear sliding table; 209 adding a liquid titration end; 210 a sample cup; 211 a reagent storage tank; 212 a reagent storage tank; 213 a reagent storage tank;
FIG. 3 is a schematic diagram of the structure of the positioning of the added liquid drop of the automatic titrator for the terminal carboxyl group content;
reference numerals: 300, positioning the liquid drop; 301 inner wall; 302 a color recognition detector; 303 a light source; 304 a homogenizing mechanism;
FIG. 4 is a schematic view of a sample storage site according to the present invention;
reference numerals: 400 sample storage locations; 401 inner wall; 402 an inductive device; 403 temperature sensor;
FIG. 5 is a schematic structural diagram of a heating reflux position of the automatic titrator for terminal carboxyl group content according to the present invention.
Reference numerals: 500 heating a reflux position; 501 heating a jacket; 502 temperature sensors; 503 a timer; 504 a gravity sensor; 505 a homogenizing mechanism;
FIG. 6 is a flow chart of titration for an automatic titrator according to the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 and fig. 2, the present embodiment provides an automatic titrator for terminal carboxyl group content, which includes a work platform 100, a sample cup moving mechanism 100A, a condensation moving mechanism 100B, and a reagent adding mechanism 100C;
the work platform 100 comprises a sample area 101, a titration solution adding area 102, a heating reflux area 103 and a condensation waiting area 104, wherein the number of sample storage positions is equal to the number of heating reflux positions.
The sample area 101 is provided with a plurality of sample storage positions 400 for storing samples to be detected; the sample storage position 400 is internally provided with a sensing device 402 for sensing the position of the sample and whether the sample exists on the position, and sending a coordinate signal of the sample to the sample cup moving mechanism 100A; the sample cup moving mechanism 100A sequentially grabs the samples according to the coordinates of the samples in the working area; the sample storage position 400 is provided with a temperature sensor for measuring the temperature of the sample.
The liquid adding titration region 102 is provided with a plurality of liquid adding drop locations 300 for storing samples to be added with liquid and titrated, the liquid adding drop locations 300 are provided with color recognition detectors 302 and light sources 303, the color recognition detectors 302 recognize colors and changes of the samples on the titration locations, when a titration end point is reached, a termination signal is sent to the reagent adding mechanism 100C, the reagent adding mechanism 100C stops adding the current reagent according to the termination signal, the liquid adding titration location 300 is provided with a homogenizing device 304, and the homogenizing device 304 is used for mixing the samples and the reagent.
The heating reflux area 103 is provided with a plurality of heating reflux positions 500 for storing samples to be heated and refluxed; the heating reflux position 500 is provided with a heating device 501, a temperature control device 502, a timer 503, a gravity sensor 504 and a homogenizing mechanism 505, and a sample can be heated and refluxed in the heating reflux area 103 according to the set temperature and time;
the sample cup moving mechanism 100A moves in the left-right direction, the front-back direction, and the up-down direction in the working platform 100, and moves the sample cup in the working platform to a designated position according to a work flow.
The sample cup moving mechanism 100A is composed of an X-axis fixing surface 201, a track 202, a Y1 axis moving arm 203 and a Z1 axis vertical moving arm 204; the moving arm 203 has a rail 202, the moving arm 203 is mounted on the X-axis fixing surface 201, and the moving arm 203 moves along the rail 202 of the fixing surface.
The Z1 axis vertical moving arm 204 is installed on the Y1 axis moving arm 203, the Z1 axis vertical moving arm 204 moves along the track on the Y1 axis moving arm 203, and the end of the Z1 axis vertical moving arm 204 is provided with a clamping mechanism which can vertically move and grab the sample cup 210 on the working platform 100.
The condensation movement mechanism 100B moves in the work platform 100 in two directions, i.e., left and right, and up and down, and moves the condensation tube 206 fixed to the movement arm 205 to the heating and reflow region 103 to be in contact with the sample cup 210.
The reagent adding mechanism 100C moves back and forth in the liquid adding titration area 102, adds specified reagents to a sample cup 210 placed in the working range of the reagent adding mechanism according to a specified work flow, comprises a single fixed arm 207 with a Y3 shaft, a linear sliding table 208, a liquid adding titration end 209 and three reagent storage tanks 211-213, and is used for storing a phenol/trichloromethane mixed solvent, a bromophenol blue indicator and a potassium hydroxide-ethanol standard titration solution.
The Y3 shaft fixing arm 207 is installed on the X shaft fixing surface 201; the linear sliding table 208 is mounted on the Y3 shaft fixing arm 207 and can slide back and forth on the linear sliding table 208, the dripping end 209 is mounted on the linear sliding table 208, the dripping end 209 is provided with three liquid inlet ends and three liquid outlet ends, and the reagent in the reagent storage tanks 211-213 enters from the liquid inlet ends and is output from the liquid outlet ends.
The titration method of the automatic titrator for the terminal carboxyl group content in the embodiment is as shown in fig. 6, and includes the following steps:
step S1, after the device is started and preheated, respectively placing the samples in the sample areas;
s2, the sample cup moving mechanism grabs the sample, moves the sample to the position of the added liquid drop through the upward movement of X, Y, Z direction, and simultaneously the reagent adding mechanism moves to the added liquid titration position to add 50mL of the phenol/trichloromethane mixed solvent;
s3, grabbing the sample to a heating reflux position, detecting whether the sample area has the sample to be detected, if so, jumping to S3, and if not, jumping to S4;
step S4, the condensation moving mechanism moves to the heating reflux area and is connected with the sample cup;
step S5, when the sample on the heating reflux position is heated to a preset temperature (such as 200 ℃), the timer starts timing, and when the heating reflux time (such as 40 min) is reached, the sample cup moving mechanism grabs the sample to the sample storage position of the sample area and cools, and the heating temperature and the heating time are set according to different samples;
step S6, after the sample on the sample storage position is cooled to the designated temperature, the sample moving mechanism moves the sample to the liquid adding titration position, and designated reagents are sequentially dripped
And step S7, judging the end point of the reagent by a visual recognition mechanism, recording the dropping amount, and calculating the terminal carboxyl group content of the sample.
In the above embodiment, the condition for the step S3 to proceed to the step S4 is that the samples are repeated until the heating reflux is full or the sample area has no sample to be tested;
when the number of the samples to be detected is less than the number of the heating reflux positions and no sample to be detected exists, continuing to perform the following steps S4-7;
when the number of the samples to be detected is larger than the number of the heating reflux positions, when the number of the heating reflux positions is full, and a sample is sent into a cooling link, a new sample is taken from the sample area, enters a liquid adding titration area and a reflux heating area, and the sequence of liquid adding and reflux is continued to be queued until the number of the samples to be detected in the working area is 0.
In another embodiment, as shown in fig. 2, the number of sample holding bits > the number of reflow bits is designed.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
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| CN116953155A (en) * | 2023-09-19 | 2023-10-27 | 泉州翔龙石化有限公司 | Method and device for determining mass fraction of aluminum chloride in polyaluminum chloride |
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