1. Maj mam ntxiv phosphorus trichloride dropwise rau dej thaum stirring; tswj tus nqi ntawm qhov sib ntxiv kom tiv thaiv cov tshuaj tiv thaiv kom tsis txhob muaj zog heev, thiab txias lub reactor siv da dej khov. Thaum ua tiav cov tshuaj tiv thaiv, lim cov sib tov. Ua kom sov cov lim dej ntawm qhov kub qis dua 140℃kom evaporate mus rau ib qho -feem peb ntawm nws cov ntim qub, yog li tshem tawm cov roj hydrogen chloride. Tom qab ntawd, txias cov tshuaj rau 60-85 degree, ntxiv me me ntawm crystalline phosphorous acid los ua cov noob muaju, thiab txuas ntxiv txias thiab nplawm kom induce crystallization, yielding phosphorous acid.
2. Siv 1000 mL peb-caj dab puag ncig- hauv qab lub raj mis thiab muab nws nrog lub tshuab nqus dej, lub qhov tso tawm, thiab lub condenser, txuas lub qhov hluav taws xob mus rau HCl nqus khoom. Muab cov dej distilled rau hauv lub khob thiab txias nrog dej khov. Thaum stirring, maj mam ntxiv 100 mL ntawm freshly distilled PCl3 (boiling ntau: 74-76 degree) los ntawm kev xa me nyuam rov funnel. Lim cov sib tov, ces evaporate lub filtrate ntawm kub hauv qab 140℃kom txog thaum nws ntim tau txo mus rau ib tug -feem peb ntawm qhov qub. Txias cov tshuaj rau 60-65 degree, nphoo rau hauv H3PO3 muaju raws li cov noob muaju, thiab txuas ntxiv txias thiab nplawm kom induce crystallization. Qhov hnyav yog kwv yees li 63 g. Txhawm rau ua kom huv ntxiv, yaj 10 g ntawm cov khoom hauv 3.5 g dej; Tom qab ntawd ntxiv cov khoom seem rau cov tshuaj no, do kom huv si, thiab sau cov muaju los ntawm kev nqus pom. Qhov hnyav yog 40 g. Khaws cov khoom rau hauv av- iav stoppered lub raj mis.
3. Siv tib lub cuab yeej raws li tau piav qhia saum toj no. Muab 300 mL ntawm CCl4 thiab 100 g ntawm freshly distilled PCl3 rau hauv lub hwj, txias qhov sib tov nrog dej khov, thiab maj mam ntxiv 75 g ntawm distilled dej dropwise los ntawm kev xa me nyuam rov funnel thaum stirring. Thaum tag nrho cov dej tau ntxiv lawm, tshem tawm cov dej khov da dej thiab txuas ntxiv mus ntxiv rau 1 teev. Hloov cov tshuaj tiv thaiv sib xyaw rau hauv qhov sib cais thiab ntxuav nws nrog plaub zaug nws qhov ntim ntawm CCl4; Yog hais tias muaj cov crystals precipitate thaum lub sij hawm txoj kev no, ntxiv 2-3 mL dej. Hloov cov tshuaj ntxuav kua qaub rau hauv lub khob los ntawm kev nqus pom siv lub iav funnel. Nyob rau hauv qhov txo qis, evaporate cov tshuaj nyob rau hauv ib da dej da dej (ntawm qhov kub tsis tshaj 60 degree) rau 3 teev kom tshem tawm HCl. Thaum kawg, muab cov khoom tso rau hauv lub desiccator kom txias thiab crystallize.
