CN113759075A - Method for detecting water content of 1-octene used for POE production - Google Patents
Method for detecting water content of 1-octene used for POE production Download PDFInfo
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- CN113759075A CN113759075A CN202111192606.6A CN202111192606A CN113759075A CN 113759075 A CN113759075 A CN 113759075A CN 202111192606 A CN202111192606 A CN 202111192606A CN 113759075 A CN113759075 A CN 113759075A
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- raw material
- octene
- water content
- poe
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- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 title claims abstract description 148
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 title claims abstract description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 76
- 238000005070 sampling Methods 0.000 claims abstract description 52
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229920006124 polyolefin elastomer Polymers 0.000 claims abstract description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 24
- 238000003825 pressing Methods 0.000 claims abstract description 16
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 238000005086 pumping Methods 0.000 claims abstract description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 31
- 238000005259 measurement Methods 0.000 abstract description 7
- 238000012827 research and development Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 16
- 239000000523 sample Substances 0.000 description 12
- 239000003054 catalyst Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229920002725 thermoplastic elastomer Polymers 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004711 α-olefin Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000010960 cold rolled steel Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012968 metallocene catalyst Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- 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
- G01N31/168—Determining water content by using Karl Fischer reagent
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of moisture content detection, and provides a method for detecting the moisture content of 1-octene used for producing POE (polyolefin elastomer), which comprises the following steps: pressing a 1-octene raw material to be detected into a raw material tank through nitrogen, wherein a circulating system is arranged in the raw material tank, discharging from the bottom of the circulating system, pumping into the top of the raw material tank through a pump, passing a pipeline in and out through a glove box, and leaving a sampling port in the glove box; before sampling, firstly starting a pump to perform tank circulation, then operating the glove box to sample, and operating a Karl Fischer instrument in the glove box to detect after sampling to obtain the water content of the 1-octene raw material. The method for detecting the water content of 1-octene solves the problem of inaccurate measurement of the water content of 1-octene at present, and accelerates the process for research and development and production of domestic POE.
Description
Technical Field
The application relates to the technical field of moisture content detection, in particular to a method for detecting the moisture content of 1-octene used for POE production.
Background
Polyolefin elastomer (POE) refers to a polymer elastomer obtained by copolymerizing ethylene-alpha olefin containing ethylene-octene copolymer, ethylene-butene copolymer and ethylene-hexene copolymer, and is mainly obtained by randomly copolymerizing 1-octene and ethylene under the action of a catalyst. POE has the properties of both rubber and thermoplastic plastics, shows high elasticity of rubber at normal temperature, can be plasticized and molded at high temperature without vulcanization, and is an important thermoplastic elastomer (TPE) raw material. Compared with other types of TPEs, POE has the advantages of better chemical resistance, lower cost for obtaining elasticity, good weather resistance, lighter weight, lower energy consumption, more environmental friendliness, and the like.
The main consumer areas of POE include: the automotive industry, the foaming industry, wires and cables, household appliances and other fields. The automobile is most applied in the automobile field, the proportion of the foaming material is more than 50%, the proportion of the foaming material is 15%, and the proportion of the foaming material is 12% in the wire and cable industry. Other fields of application include household appliances, films (including food packaging and industrial packaging), and the like, wherein the ratio is respectively 5%, 6% and 6%. At present, POE production enterprises around the world probably have 6 families, which are distributed in North America, Western Europe, Japan, Korea, Singapore, Saite and the like; the global overall capacity is about 100 million tons.
POE was first commercialized by Dow chemical company in the United states, who used a high temperature solution polymerization process, and in 1993, POE was first introduced as an ethylene/alpha-olefin random copolymer elastomer synthesized by constrained geometry metallocene catalyst (CGC catalyst for short). Compared with a Z-N catalyst, the CGC catalyst has the advantages of single active center, high catalytic efficiency and the like, but the catalyst is extremely sensitive to water, and the polymerization reaction is difficult to carry out if trace water in ppm level exists in raw materials, auxiliary materials or a reaction system. Therefore, when using CGC catalyst to prepare POE, it is necessary to detect and remove water contained in the olefin feedstock, and it is usually necessary to remove the water content of 1-octene to less than 5ppm by molecular sieve adsorption or sodium distillation. At present, in the process of detecting the water content of 1-octene, a general method is to take off-line after sampling and measure by using a Karl Fischer apparatus, but the existing off-line detection method has the problem of inaccurate measurement of the water content of 1-octene, and the POE production efficiency is seriously influenced.
Disclosure of Invention
In view of this, the application provides a method for detecting the water content of 1-octene used for producing POE, and the method has high accuracy for detecting the water content of 1-octene and is simple and convenient to operate.
The invention provides a method for detecting the water content of 1-octene used for producing POE (polyolefin elastomer), which comprises the following steps:
pressing a 1-octene raw material to be detected into a raw material tank through nitrogen, wherein a circulating system is arranged in the raw material tank, discharging from the bottom of the circulating system, pumping into the top of the raw material tank through a pump, passing a pipeline in and out through a glove box, and leaving a sampling port in the glove box;
before sampling, firstly starting a pump to perform tank circulation, then operating the glove box to sample, and operating a Karl Fischer instrument in the glove box to detect after sampling to obtain the water content of the 1-octene raw material.
In a preferred embodiment of the invention, high-purity nitrogen is used for pressurizing to 10-100 KPa, and the 1-octene raw material to be tested is pressed into a raw material tank through a pipeline.
In a preferred embodiment of the present invention, the raw material tank is constantly kept at a positive pressure of a high purity nitrogen atmosphere, and the pressure is 0.05 to 0.5 MPa.
In a preferred embodiment of the invention, the volume of the 1-octene raw material to be measured pumped by the pump of the circulating system per hour is 2-20 times of the volume of the raw material tank.
In a preferred embodiment of the invention, sampling is carried out after the 1-octene raw material to be measured circulates in the tank for 20-60 min.
In a preferred embodiment of the invention, the sampling amount of the 1-octene raw material to be detected is 10-30 mL, and the sampling amount of the Karl Fischer apparatus is 0.5-5 mL.
The invention provides a method for detecting the water content of 1-octene used for producing POE (polyolefin elastomer), which solves the problem of inaccurate measurement of the water content of 1-octene at present, and comprises the following steps: pressing a 1-octene raw material to be detected into a raw material tank through nitrogen, wherein a circulating system is arranged in the raw material tank, discharging from the bottom of the circulating system, pumping into the top of the raw material tank through a pump, passing a pipeline in and out through a glove box, and leaving a sampling port in the glove box; before sampling, firstly starting a pump to perform tank internal circulation to ensure that materials at the upper part, the middle part and the lower part are uniform, then operating sampling in a glove box, and operating a Karl Fischer instrument in the glove box to perform water content detection after sampling. The method has high accuracy in detecting the water content of the 1-octene, is simple and convenient to operate, and accelerates the process for the research and development and production of the domestic POE.
Detailed Description
The technical solutions in the embodiments of the present application are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. 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 application.
The application provides a method for detecting the water content of 1-octene used for producing POE, which comprises the following steps:
pressing a 1-octene raw material to be detected into a raw material tank through nitrogen, wherein a circulating system is arranged in the raw material tank, discharging from the bottom of the circulating system, pumping into the top of the raw material tank through a pump, passing a pipeline in and out through a glove box, and leaving a sampling port in the glove box;
before sampling, firstly starting a pump to perform tank circulation, then operating the glove box to sample, and operating a Karl Fischer instrument in the glove box to detect after sampling to obtain the water content of the 1-octene raw material.
At present, in the sampling process of the water content detection method and the sampling process of the Karl Fischer instrument, because the used apparatus and the 1-octene can contact with air, water in the air enters the 1-octene to be detected, and the detected water content is higher than the actual water content. The invention provides the method for detecting the water content of the 1-octene used for producing the POE, which can solve the problem of inaccurate measurement of the water content of the 1-octene at present and is beneficial to accelerating the research, development and production of the domestic POE.
According to the embodiment of the invention, purchased barreled 1-octene is taken as a detection object, a 1-octene raw material to be detected is connected with a material pressing system, and the 1-octene raw material enters a raw material tank through nitrogen material pressing. In the embodiment of the invention, high-purity nitrogen can be used to pressurize to 10-100 KPa according to the material of the purchased 1-octene raw material barrel, for example, the raw material barrel made of cold-rolled steel can resist 100 KPa; preferably, the nitrogen pressure is set to be 20kPa to 70kPa, and the 1-octene raw material to be tested is pressed into a raw material tank through a pipeline. In some preferred embodiments, the nitrogen pressure is set at 50 KPa.
The raw material tank is provided with a circulating system, the raw material is discharged from the bottom and is pumped into the top of the raw material tank through a pump, a pipeline enters and exits through a glove box, and a sampling port is reserved in the glove box. In the embodiment of the invention, the raw material tank keeps positive pressure of high-purity nitrogen atmosphere at all times, and the pressure is 0.05-0.5 MPa; after the pressing is finished, the nitrogen sealing pressure of the raw material tank is preferably 0.05 MPa-0.4 MPa.
Before sampling, the embodiment of the invention opens a circulation flow, firstly, the pump is started to carry out in-tank circulation, on one hand, the materials in the tank are uniformly mixed, on the other hand, the materials in the pump and the materials in the barrel are fully replaced, and the delivered sample is guaranteed to be representative. In a preferred embodiment of the invention, the volume of the 1-octene raw material to be measured pumped by the pump of the circulating system per hour is 2-20 times, preferably 5-20 times of the volume of the raw material tank.
And circulating the 1-octene raw material tank to be tested for 20-60 min, wherein the circulation time is preferably 30-60 min, and sampling is carried out after a sampling port is replaced. The method of the invention is not affected by the sampling method and can sample after replacement.
In the specific embodiment of the invention, the sampling amount of the 1-octene raw material to be detected can be 10-30 mL, and preferably 20-30 mL. After sampling, the embodiment of the invention operates a Karl Fischer apparatus in a glove box to detect the water content; specifically, the sampling needle can be replaced for more than three times for sampling detection, the sampling amount of the Karl Fischer apparatus can be 0.5-5 mL, the determination is repeated for more than 3 times, and the average value is taken to obtain the water content detection result of the 1-octene raw material.
The present invention is not particularly limited to the Karl Fischer apparatus used; the Karl Fischer instrument is used for measuring water content, and the Karl Fischer method is proposed in 1935 by adopting I2、SO2Pyridine, anhydrous CH3OH (water content below 0.05%) is prepared into reagent, the water equivalent of the reagent is measured, and the reagent are mixedAfter the reaction of the water in the sample, the water content in the sample is calculated by calculating the reagent consumption.
According to the embodiment of the invention, through the method for measuring the water content of 1-octene used by POE, the detection result is basically consistent with the online detection method, the problem that the current offline measurement of the water content of 1-octene is inaccurate is solved, and the method is beneficial to subsequent production and application.
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
Example 1
Connecting the purchased 0603 batches of barreled 1-octene with a material pressing system, setting the nitrogen pressure to be 50KPa, pressing the 1-octene raw material into a raw material tank by using high-purity nitrogen, and setting the nitrogen sealing pressure of the raw material tank to be 0.05MPa after the 1-octene raw material is finished; opening a circulation flow, starting a pump, wherein the volume of 1-octene pumped by the circulation pump per hour is 10 times of that of the raw material tank, and the circulation time is 30 min; and (3) replacing the sampling port, then sampling, namely sampling 30mL, replacing the sampling needle for more than three times, detecting by using an MKC-710M Karl Fischer instrument, repeatedly measuring for three times, and taking an average value, wherein the details are shown in Table 1.
Example 2
Connecting the purchased 0603 batches of barreled 1-octene with a material pressing system, setting the nitrogen pressure to be 50KPa, pressing the 1-octene raw material into a raw material tank by using high-purity nitrogen, and setting the nitrogen sealing pressure of the raw material tank to be 0.4MPa after the 1-octene raw material is finished; opening a circulation flow, starting a pump, wherein the volume of 1-octene pumped by the circulation pump per hour is 20 times of that of the raw material tank, and the circulation time is 60 min; and (3) replacing the sampling port, then sampling, namely sampling 30mL, replacing the sampling needle for more than three times, detecting by using a Karl Fischer instrument, repeatedly measuring for three times, and taking an average value, wherein the details are shown in Table 1.
Example 3
Connecting the purchased 0605 batches of barreled 1-octene with a material pressing system, setting the nitrogen pressure to be 50KPa, pressing the 1-octene raw material into a raw material tank by using high-purity nitrogen, and setting the nitrogen sealing pressure of the raw material tank to be 0.4MPa after the 1-octene raw material is finished; opening a circulation flow, starting a pump, wherein the volume of 1-octene pumped by the circulation pump per hour is 20 times of that of the raw material tank, and the circulation time is 60 min; and (3) replacing the sampling port, then sampling, namely sampling 30mL, replacing the sampling needle for more than three times, detecting by using a Karl Fischer instrument, repeatedly measuring for three times, and taking an average value, wherein the details are shown in Table 1.
Comparative example
Connecting the purchased 0603 batches of barreled 1-octene with a material pressing system, setting the nitrogen pressure to be 50KPa, pressing the 1-octene raw material into a raw material tank by using high-purity nitrogen, and setting the nitrogen sealing pressure of the raw material tank to be 0.05MPa after the 1-octene raw material is finished; sampling is carried out after a sampling port without replacement, 30mL of the sample is taken, a sampling needle is replaced for more than three times, the MKC-710M Karl Fischer instrument is subjected to sample injection detection, the sample injection amount is 50 mu L, the measurement is repeated for three times, and the average value is obtained and is detailed in Table 1.
Different numbers of 1-octene indicate different batches of purchased materials, 1-octene with the same number and different numbers are respectively compared with detection accuracy by using the method, the online detection method and the general offline detection method, and the experimental results are shown in Table 1. The on-line detection method is that the liquid is conveyed to an on-line analysis probe through a tank bottom pump and then flows back to the tank; the off-line detection method comprises the steps of sampling from the bottom of the tank to a sampling bottle, and injecting the sampling bottle into a Karl Fischer apparatus for detection.
Table 1: detection result of water content of 1-octene
Remarking: the online detection also has certain errors because the pump flow is not stable, the feeding amount fluctuates, and the detection value fluctuates in a certain interval. The offline detection value is greatly influenced by the moisture content in the air; the comparative examples without replacement have a deviation.
According to table 1, the water content of the off-line detection method is affected by the sampling method, and the detection result has a large deviation compared with the on-line detection method; the method of the invention is not influenced by the sampling method and can sample after replacement, so the method is basically consistent with the online detection method.
According to the method of the invention, the water content of Karl Fischer is calibrated by injecting standard water, each injection is 0.1 mu L, the Karl Fischer is set to have a sample size of 1mL, and the repeatability is shown in Table 2.
Table 2: karl Fischer water content measurement
| Number of detections | Measured value/ppm | Deviation of |
| First time of detection | 101.5 | 0.36％ |
| To secondary detection | 102.4 | 0.52％ |
| Third time of detection | 101.7 | 0.17％ |
From table 2, it can be found that the difference between the three detection values is not large, and the experimental deviation is in a reliable range, so that the karl fischer instrument and the detection method thereof are feasible. In conclusion, the method has high accuracy in detecting the water content of the 1-octene, and is simple and convenient to operate.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. A method for detecting the water content of 1-octene used for producing POE is characterized by comprising the following steps:
pressing a 1-octene raw material to be detected into a raw material tank through nitrogen, wherein a circulating system is arranged in the raw material tank, discharging from the bottom of the circulating system, pumping into the top of the raw material tank through a pump, passing a pipeline in and out through a glove box, and leaving a sampling port in the glove box;
before sampling, firstly starting a pump to perform tank circulation, then operating the glove box to sample, and operating a Karl Fischer instrument in the glove box to detect after sampling to obtain the water content of the 1-octene raw material.
2. The method for detecting the water content of 1-octene used in POE production according to claim 1, wherein the 1-octene raw material to be detected is pressed into a raw material tank through a pipeline by pressurizing to 10-100 KPa with high-purity nitrogen.
3. The method for detecting the water content of 1-octene used in POE production according to claim 1, wherein the pressure of the raw material tank is constantly kept at a positive pressure of high-purity nitrogen atmosphere, and the pressure is 0.05-0.5 MPa.
4. The method for detecting the water content of 1-octene used in the production of POE according to claim 1, wherein a volume of 1-octene raw material to be detected pumped by a pump of the circulating system per hour is 2-20 times of a volume of a raw material tank.
5. The method for detecting the water content of 1-octene used for producing POE (polyolefin elastomer) according to claim 1, wherein the 1-octene to be detected is sampled after circulating in the raw material tank for 20-60 min.
6. The method for detecting the water content of 1-octene used in the production of POE according to any one of claims 1 to 5, wherein the sample volume of 1-octene raw material to be detected is 10-30 mL, and the sample volume of Karl Fischer apparatus is 0.5-5 mL.
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- 2021-10-13 CN CN202111192606.6A patent/CN113759075A/en active Pending
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