CN110156565A - Trimethylolpropane extraction and water washing method - Google Patents
Trimethylolpropane extraction and water washing method Download PDFInfo
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- CN110156565A CN110156565A CN201910583562.6A CN201910583562A CN110156565A CN 110156565 A CN110156565 A CN 110156565A CN 201910583562 A CN201910583562 A CN 201910583562A CN 110156565 A CN110156565 A CN 110156565A
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- 238000005406 washing Methods 0.000 title claims abstract description 73
- 238000000605 extraction Methods 0.000 title claims abstract description 61
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 title claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000012071 phase Substances 0.000 claims abstract description 120
- 239000004280 Sodium formate Substances 0.000 claims abstract description 31
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims abstract description 31
- 235000019254 sodium formate Nutrition 0.000 claims abstract description 31
- 239000012074 organic phase Substances 0.000 claims abstract description 15
- 238000004064 recycling Methods 0.000 claims abstract description 8
- 239000000284 extract Substances 0.000 claims abstract description 5
- 238000004853 microextraction Methods 0.000 claims description 43
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical group CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 26
- 239000012141 concentrate Substances 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 7
- 229910001415 sodium ion Inorganic materials 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 239000012847 fine chemical Substances 0.000 abstract 1
- 238000005191 phase separation Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 10
- 239000006227 byproduct Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000012850 discrimination method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 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 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- YYKMQUOJKCKTSD-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanal Chemical compound CCC(CO)(CO)C=O YYKMQUOJKCKTSD-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000005705 Cannizzaro reaction Methods 0.000 description 1
- 238000005575 aldol reaction Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 235000013847 iso-butane Nutrition 0.000 description 1
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- NUBTXWNDDOMQPK-UHFFFAOYSA-N pentane-1,1,2-triol Chemical compound CCCC(O)C(O)O NUBTXWNDDOMQPK-UHFFFAOYSA-N 0.000 description 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N sec-butylidene Natural products CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- -1 trihydroxy methyl Chemical group 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of fine chemical engineering, and particularly discloses a trimethylolpropane extraction and washing method, which comprises the following steps: and (3) extraction: extracting and separating trimethylolpropane by using a first micro-extractor to obtain an extract phase and a raffinate phase; washing with water: pumping the extracted phase and pure water into a second micro-extractor for primary washing and phase splitting to separate a first oil phase and a first water phase; the first water phase enters a first micro extractor, and the first oil phase enters a third micro extractor for secondary washing and phase separation, and is divided into a second water phase and a second oil phase again; the second water phase returns to the second micro-extractor for recycling, and the second oil phase obtains an organic phase containing sodium formate. The extraction and water washing method adopts a micro-channel extraction technology, and performs extraction and water washing on the trimethylolpropane for a plurality of times through the micro-extractor, so that the method has the advantages of convenient operation by personnel, low production energy consumption, convenient equipment heat preservation, low production cost and convenient realization, and the obtained product is superior to the traditional process.
Description
Technical field
The invention belongs to technical field of fine, the method for specifically a kind of trimethylolpropane extraction washing.
Background technique
Trimethylolpropane, alias are 2-2 dihydroxymethyl butanol, and molecular formula C6H14O3, No. CAS is 77-99-6, phase
To molecular mass 134.17.Trimethylolpropane is mainly used for alkyd resin, polyurethane, unsaturated-resin, polyester resin, coating
Equal fields are used for modifier and crosslinking agent for the manufacture of composite solidpropellant powder charge clad and heat insulation layer.Three hydroxyls
Methylpropane night can be used for synthesizing aeroengine oil, printing ink etc., and trimethylolpropane also acts as textile auxiliary and polychlorostyrene
The heat stabilizer of vinyl.
There are mainly two types of the synthetic methods of trimethylolpropane: condensation discrimination method and condensation hydrogenation method.Being condensed discrimination method is
Traditional two-step synthesis method, this technics comparing is mature, but by-product is more, needs to consume a large amount of alkali, formaldehyde consumption is big, cost
It is high.Condensation hydrogenation method is the two-step method to grow up the nineties, is first condensed repeated hydrogenation, can save the formaldehyde of one third and big
The alkali of amount, by-product is relatively fewer, and purification is relatively simple, and equipment is few, at low cost, but this method to hydrogenation plant and is urged
Agent is more demanding, is suitble to continuous production.
Condensation discrimination method is divided into calcium method and sodium method again.Wherein sodium method is i.e. using n-butanal and formaldehyde as raw material, with sodium hydroxide
For catalyst, aldol reaction is carried out at a lower temperature and generates 2,2- dihydroxymethyl butyraldehyde, then with excessive formaldehyde and by force
Alkali effect occurs Cannizzaro reaction and generates trimethylolpropane.Reaction equation are as follows:
Production process is (as shown in Figure 1): by the way that by n-butanal and formaldehyde, after condensation reaction generates liquid concentration, use is molten
After agent extraction, washing, the trimethylolpropane extracting solution for being substantially free of sodium formate is obtained, extracting solution obtains after desolventizing
Thick trimethylolpropane, thick trimethylolpropane are refined under a high vacuum again after first sloughing light component under a high vacuum, are obtained
To qualified liquid trimethylolpropane.Sheet trimethylolpropane finished product is made by flaker in liquid trimethylolpropane.
At present in Conventional process, extraction washes extract using large-scale extraction tower, water scrubber and washes behaviour
Make, the device is complicated, operating process condition is harsh, insulation of equipment is difficult, production process energy consumption is high, high production cost.
Summary of the invention
The object of the present invention is to provide a kind of methods of trimethylolpropane extraction washing, can be widely used in large-scale industry
In production, mainly solving trimethylolpropane extraction washing in the prior art, the device is complicated, operating process condition is harsh, equipment is protected
The problem of Wen Nan, production process energy consumption height, high production cost.
In order to solve the above technical problems, the present invention provides a kind of methods of trimethylolpropane extraction washing, including with
Lower step:
The extraction of S1, trimethylolpropane:
Concentrate containing trimethylolpropane and extractant are proportionally added in the first micro-extraction apparatus;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;
Raffinate phase enters sodium formate process units, and extraction phase enters washing step;
The washing of S2, trimethylolpropane:
Extraction phase and pure water are proportionally passed through into metering pump and squeeze into the second micro-extraction apparatus progress once washing, split-phase, point
First oil phase and the first water phase out;
The first water phase that once washing, split-phase are got enters in the first micro-extraction apparatus, and the first oil mutually enters the micro- extraction of third
Progress secondary washing, split-phase in device is taken, the second water phase and the second oily phase are again broken down into;
The second water phase that secondary washing, split-phase are got returns to recycling and reusing in the second micro-extraction apparatus, the second oily phase
The organic phase for being substantially free of sodium formate is obtained, the sodium ions content in organic phase is measured.
Specifically, extractant is octanol in the S1.
Further, the ratio of the concentrate and extractant is 1:22~2.5.
Further, the ratio of extraction phase and pure water is 1:0.04~0.06 in the S2.
Specifically, the first oil mutually includes trimethylolpropane, extractant octanol and heavy component in the S2.
Specifically, the organic phase of the second oily phase includes trimethylolpropane, extractant octanol and heavy component in the S2.
The beneficial effects of the present invention are: the method for trimethylolpropane extraction washing of the present invention extracts skill using microchannel
Art carries out extraction, washing several times to trimethylolpropane by simple equipment micro-extraction apparatus, reduces the organic phase of extraction
In impurity content, improve the yield of trimethylolpropane, but also have personnel easy to operate, production energy consumption is low, and equipment is protected
The characteristics of temperature is convenient, and production cost is low, is easy to implement, and obtained product is better than traditional handicraft.
Detailed description of the invention
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical solution of the present invention
The attached drawing used is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, right
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings
Its attached drawing.
Fig. 1 is the flow sheet of trimethylolpropane in background technique;
Fig. 2 is the extraction of trimethylolpropane of the invention, washing process figure.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
In an embodiment of the present invention, a kind of method for specifically disclosing trimethylolpropane extraction washing, including it is following
Step:
The extraction of S1, trimethylolpropane:
First micro- extraction is added according to the ratio of 1:22~2.5 in concentrate containing trimethylolpropane and extractant octanol
It takes in device;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;
Raffinate phase enters sodium formate process units, and extraction phase enters washing step;
The washing of S2, trimethylolpropane:
Extraction phase and pure water are squeezed into the second micro-extraction apparatus by metering pump according to the ratio of 1:0.04~0.06 and carry out one
Secondary washing, split-phase separate the first oil phase and the first water phase;
The first water phase that once washing, split-phase are got enters in the first micro-extraction apparatus, and the first oil mutually enters the micro- extraction of third
Progress secondary washing, split-phase in device is taken, is again broken down into the second water phase and the second oily phase, first oil mutually includes trihydroxy methyl third
Alkane, extractant octanol and heavy component;
The second water phase that secondary washing, split-phase are got returns to recycling and reusing in the second micro-extraction apparatus, the second oily phase
The organic phase for being substantially free of sodium formate is obtained, the sodium ions content in organic phase is measured, the organic phase of the described second oily phase includes
Trimethylolpropane, extractant octanol and heavy component.
Embodiment 1:
The extraction process of S1, trimethylolpropane:
Concentrate and extractant octanol are squeezed into the first micro-extraction apparatus by metering pump according to 1:2.2 ratio;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;Raffinate phase is contained
The seldom aqueous sodium formate solution of machine object amount enters traditional sodium formate process units, measures content of organics therein and is
0.076%, raw material is provided to carry out the production of byproduct sodium formate, guarantees sodium formate product by measuring wherein content of organics
Quality, because high organic content will affect the quality of sodium formate product;
Extraction phase carries out the processing of next step water-washing process, and raffinate phase carries out waste treatment;
S2, water-washing process:
Extraction phase and pure water be driven into the second micro-extraction apparatus according to 1:0.05 ratio by metering pump carry out once washing,
Split-phase;
The first water phase that once washing, split-phase are got enters the first micro-extraction apparatus and carries out extracting operation again, once washing,
The first oil that split-phase is got mutually enters third micro-extraction apparatus and carries out secondary washing, split-phase;
The second water phase that secondary washing, split-phase are got is used back to the recycling of the second micro-extraction apparatus;Secondary washing, split-phase point
The second oil obtained mutually obtains the organic phase seldom containing sodium formate, and measuring sodium ions content therein is 54ppm.
Embodiment 2
The extraction process of S1, trimethylolpropane:
Concentrate and extractant octanol are squeezed into the first micro-extraction apparatus by metering pump according to 1:2.3 ratio;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;Raffinate phase is contained
The seldom aqueous sodium formate solution of machine object amount enters traditional sodium formate process units, measures content of organics therein and is
0.078%, raw material is provided to carry out the production of byproduct sodium formate, guarantees sodium formate product by measuring wherein content of organics
Quality, because high organic content will affect the quality of sodium formate product;
Extraction phase carries out the processing of next step water-washing process, and raffinate phase carries out waste treatment;
S2, water-washing process:
Extraction phase and pure water be driven into the second micro-extraction apparatus according to 1:0.05 ratio by metering pump carry out once washing,
Split-phase;
The first water phase that once washing, split-phase are got enters the first micro-extraction apparatus and carries out extracting operation again, once washing,
The first oil that split-phase is got mutually enters third micro-extraction apparatus and carries out secondary washing, split-phase;
The second water phase that secondary washing, split-phase are got is used back to the recycling of the second micro-extraction apparatus;Secondary washing, split-phase point
The second oil obtained mutually obtains the organic phase for being substantially free of sodium formate, and measuring sodium ions content therein is 36ppm.
Embodiment 3
The extraction process of S1, trimethylolpropane:
Concentrate and extractant octanol are squeezed into the first micro-extraction apparatus by metering pump according to 1:2.4 ratio;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;Raffinate phase is contained
The seldom aqueous sodium formate solution of machine object amount enters traditional sodium formate process units, measures content of organics therein and is
0.085%, raw material is provided to carry out the production of byproduct sodium formate, guarantees sodium formate product by measuring wherein content of organics
Quality, because high organic content will affect the quality of sodium formate product;
Extraction phase carries out the processing of next step water-washing process, and raffinate phase carries out waste treatment;
S2, water-washing process:
Extraction phase and pure water be driven into the second micro-extraction apparatus according to 1:0.05 ratio by metering pump carry out once washing,
Split-phase;
The first water phase that once washing, split-phase are got enters the first micro-extraction apparatus and carries out extracting operation again, once washing,
The first oil that split-phase is got mutually enters third micro-extraction apparatus and carries out secondary washing, split-phase;
The second water phase that secondary washing, split-phase are got is used back to the recycling of the second micro-extraction apparatus;Secondary washing, split-phase point
The second oil obtained mutually obtains the organic phase for being substantially free of sodium formate, and measuring sodium ions content therein is 18ppm.
Embodiment 4
The extraction process of S1, trimethylolpropane:
Concentrate and extractant octanol are squeezed into the first micro-extraction apparatus by metering pump according to 1:2.5 ratio;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;Raffinate phase is contained
The seldom aqueous sodium formate solution of machine object amount enters traditional sodium formate process units, measures content of organics therein and is
0.069%, raw material is provided to carry out the production of byproduct sodium formate, guarantees sodium formate product by measuring wherein content of organics
Quality, because high organic content will affect the quality of sodium formate product;
Extraction phase carries out the processing of next step water-washing process, and raffinate phase carries out waste treatment;
S2, water-washing process:
Extraction phase and pure water be driven into the second micro-extraction apparatus according to 1:0.05 ratio by metering pump carry out once washing,
Split-phase;
The first water phase that once washing, split-phase are got enters the first micro-extraction apparatus and carries out extracting operation again, once washing,
The first oil that split-phase is got mutually enters third micro-extraction apparatus and carries out secondary washing, split-phase;
The second water phase that secondary washing, split-phase are got is used back to the recycling of the second micro-extraction apparatus;Secondary washing, split-phase point
The second oil obtained mutually obtains the organic phase for being substantially free of sodium formate, and measuring sodium ions content therein is 14ppm.
Microchannel abstraction technique compared with traditional handicraft compared with:
Above disclosed be only a kind of preferred embodiment of the invention, cannot limit the present invention's certainly with this
Interest field, therefore equivalent changes made in accordance with the claims of the present invention, are still within the scope of the present invention.
Claims (6)
1. a kind of method of trimethylolpropane extraction washing, which comprises the following steps:
The extraction of S1, trimethylolpropane:
Concentrate containing trimethylolpropane and extractant are proportionally added in the first micro-extraction apparatus;
Trimethylolpropane obtains extraction phase with raffinate phase after the first micro-extraction apparatus extraction and separation;
Raffinate phase enters sodium formate process units, and extraction phase enters washing step;
The washing of S2, trimethylolpropane:
It extraction phase and pure water is proportionally passed through into metering pump squeezes into the second micro-extraction apparatus and carry out once washing, split-phase, separate the
One oil phase and the first water phase;
The first water phase that once washing, split-phase are got enters in the first micro-extraction apparatus, and the first oil mutually enters third micro-extraction apparatus
Middle progress secondary washing, split-phase are again broken down into the second water phase and the second oily phase;
The second water phase that secondary washing, split-phase are got mutually is obtained back to recycling and reusing in the second micro-extraction apparatus, the second oil
Organic phase measures the sodium ions content in organic phase.
2. a kind of method of trimethylolpropane extraction washing according to claim 1, which is characterized in that extract in the S1
Taking agent is octanol.
3. a kind of method of trimethylolpropane extraction washing according to claim 2, which is characterized in that the concentrate
Ratio with extractant is 1:22~2.5.
4. a kind of method of trimethylolpropane extraction washing according to claim 1, which is characterized in that extract in the S2
Taking mutually is 1:0.04~0.06 with the ratio of pure water.
5. a kind of method of trimethylolpropane extraction washing according to claim 1, which is characterized in that the in the S2
One oil mutually includes trimethylolpropane, extractant octanol and heavy component.
6. a kind of method of trimethylolpropane extraction washing according to claim 1, which is characterized in that the in the S2
The organic phase of two oily phases includes trimethylolpropane, extractant octanol and heavy component.
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CN110563562A (en) * | 2019-09-25 | 2019-12-13 | 南通百川新材料有限公司 | extraction and water washing method of trimethylolpropane heavy component |
CN110563562B (en) * | 2019-09-25 | 2022-08-02 | 南通百川新材料有限公司 | Extraction and water washing method of trimethylolpropane heavy component |
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