SU165697A1 - METHOD OF OBTAINING MEDIUM PHOSPHITES AND PULPHOSPHOSPHINICS - Google Patents
METHOD OF OBTAINING MEDIUM PHOSPHITES AND PULPHOSPHOSPHINICSInfo
- Publication number
- SU165697A1 SU165697A1 SU740023A SU740023A SU165697A1 SU 165697 A1 SU165697 A1 SU 165697A1 SU 740023 A SU740023 A SU 740023A SU 740023 A SU740023 A SU 740023A SU 165697 A1 SU165697 A1 SU 165697A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- phosphites
- pulphosphosphinics
- obtaining medium
- cellulose
- medium
- Prior art date
Links
- AQSJGOWTSHOLKH-UHFFFAOYSA-N Phosphite Chemical compound [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 title description 4
- 229920002678 cellulose Polymers 0.000 description 7
- 239000001913 cellulose Substances 0.000 description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 239000002904 solvent Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 4
- ABLZXFCXXLZCGV-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 125000005538 phosphinite group Chemical group 0.000 description 2
- 238000006366 phosphorylation reaction Methods 0.000 description 2
- 230000000865 phosphorylative Effects 0.000 description 2
- ABLZXFCXXLZCGV-UHFFFAOYSA-L CHEBI:8154 Chemical class [O-]P([O-])=O ABLZXFCXXLZCGV-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000000749 insecticidal Effects 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
Description
Известен способ получени фосфитов и фосфииитов целлюлозы, заключающийс в том, что переэтерификацию эфиров кислот трехвалентного фосфора с целлюлозой провод т в присутствии металлического натри . A method of producing phosphites and phosphonates of cellulose is known, which consists in that the transesterification of trivalent phosphorus acid esters with cellulose is carried out in the presence of metallic sodium.
Однако известный способ сложен по выполнению .However, the known method is difficult to implement.
Предлагаетс более простой способ получени средних фосфитов и фосфинитов целлюлозы , особенность которого состоит в том, что фосфорилирование целлюлозы провод т фосфористой кислотой В присутствии растворител - димет1илформамида - или без него.A simpler method is proposed for obtaining medium phosphites and cellulose phosphinites, the peculiarity of which is that phosphorylation of cellulose is carried out with phosphorous acid. In the presence of a solvent, dimethyl formamide, with or without it.
Полученные продукты примен ютс при синтезе полимерных инсектицидов.The products obtained are used in the synthesis of polymeric insecticides.
Пример. К 4 г сухой целлюлозы добавл ют 300 мл Зо/о-ного раствора фосфористой кислоты в диметилформамиде и в токе азота отгон ют 40 мл растворител под вакуумом 200 мм при температуре бани 130° С. Затем Example. To 4 g of dry cellulose, 300 ml of a Zo / about-aqueous solution of phosphorous acid in dimethylformamide is added and 40 ml of solvent under a vacuum of 200 mm are distilled off at a bath temperature of 130 ° C. Then
в реакционную смесь добавл ют 40 мл толуола и продолжают нагревание без вакуума при температуре бани 155-160°С с отгонкой растворител .40 ml of toluene are added to the reaction mixture and heating is continued without vacuum at a bath temperature of 155-160 ° C with distillation of the solvent.
Нагревание ведут в течение 20 час, после чего растворитель сливают, а целлюлозу декантируют сначала толуолом (2x50 мл, затем диметилформамидом (5X50 мл); после этого продукт фильтруют или центрифугируют , промывают метанолом (2X50 мл) и сушат .Heating is carried out for 20 hours, after which the solvent is drained and the cellulose is decanted first with toluene (2x50 ml, then dimethylformamide (5X50 ml); then the product is filtered or centrifuged, washed with methanol (2X50 ml) and dried.
Предмет изобретени Subject invention
Способ получени средних фосфитов и фосфинитов целлюлозы фосфорилированием ее фосфорсодержащими соединени ми, отличающийс тем, что, с целью упрощени способа, в качестве фосфорсодержащего соединени примен ют фосфористую кислоту.The method of producing medium phosphites and phosphinites of cellulose by phosphorylation of phosphorus-containing compounds with it, characterized in that, in order to simplify the process, phosphorous acid is used as the phosphorus-containing compound.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU165697A1 true SU165697A1 (en) |
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