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id="9jlc8z4" class="font"> 偶氮二異庚腈生產(chǎn)工藝改進(jìn)的制作方法 </div> </h1> </div> </div> <ul class="e_box p_dataSource borderT_default" data-ename="資訊信息"> <li id="ndp4n8t" class="sort"><span id="8pb4ace" class="i_sort">分類(lèi)：</span><a href="/news/2/">行業(yè)新聞</a></li> <li id="zelsuwt" class="auth"><span id="dh39ah4" class="i_auth">作者：</span></li> <li id="agsz4j9" class="source"><span id="rkw9fmt" class="i_source">來(lái)源:</span></li>  <li id="bmtq4ln" class="date"><span id="in9b39p" class="i_pubDate">時(shí)間:</span>2020-10-20</li> <li id="ddfrvsk" class="pvs"><span id="fa4qkme" class="i_pvs">訪(fǎng)問(wèn)量：</span><span id="9covxeg" class="p_viewCount">0</span></li> </ul>  <p class="e_article p_summary background_info" data-ename="資訊概要信息"> <span><span id="4n4oqxe" class="i_SummaryBox">[Description]</span></span>專(zhuān)利名稱(chēng)：偶氮二異庚腈生產(chǎn)工藝改進(jìn)的制作方法　　技術(shù)領(lǐng)域：　　本發(fā)明屬于偶氮化合物生產(chǎn)工藝?！　∨嫉惛妗灿置?·2′-偶氮(2·4-二甲基戊腈)〕是一種常用的高分子聚合引發(fā)劑。它的引發(fā)效率高，反應平穩，聚合產(chǎn)物質(zhì)量?jì)?yōu)，在聚氯乙烯生產(chǎn)中的應用尤為普遍。目前生產(chǎn)偶氮二異庚腈的工藝路線(xiàn)有二種一種是由甲基異丁基甲酮與肼反應生成己酮連氮，用氰氫酸氰化為二異庚腈肼，再用氯氣氧化為偶氮二異庚腈，該工藝氰化 </p>  </div>  <div id="bry3n44" class="e_box p_imgsBox borderB_default"> <div id="qbdkmtv" class="swiper-container gallery-top"> <div id="dyfc3jq" class="swiper-wrapper"> <div data-foreachitem class="swiper-slide"> <img src="http://img202.yun300.cn/repository/image/TtHCDkS-SdKWlX4uWvYaBQ.jpg_{i}xaf.jpg?tenantId=208134&viewType=1" class='js_thumb' title='' alt='news' /> <div id="jegn4zl" class="e_box p_SummaryBox background_shade"> <div id="z98qsuw" class="e_box p_textBoxs color_horizon"> <h4 class="e_title p_ImgHead color_horizon" data-ename="圖片標題"></h4> <p class="e_article p_ImgSummary color_horizon" data-ename="圖片描述"></p> </div> </div> </div> </div>  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</div> </h1> </div> </div>  <p class="e_article p_summary" data-ename="資訊概要信息"> <span><span id="ss93gi9" class="i_SummaryBox">[Description]</span></span>專(zhuān)利名稱(chēng)：偶氮二異庚腈生產(chǎn)工藝改進(jìn)的制作方法　　技術(shù)領(lǐng)域：　　本發(fā)明屬于偶氮化合物生產(chǎn)工藝?！　∨嫉惛妗灿置?·2′-偶氮(2·4-二甲基戊腈)〕是一種常用的高分子聚合引發(fā)劑。它的引發(fā)效率高，反應平穩，聚合產(chǎn)物質(zhì)量?jì)?yōu)，在聚氯乙烯生產(chǎn)中的應用尤為普遍。目前生產(chǎn)偶氮二異庚腈的工藝路線(xiàn)有二種一種是由甲基異丁基甲酮與肼反應生成己酮連氮，用氰氫酸氰化為二異庚腈肼，再用氯氣氧化為偶氮二異庚腈，該工藝氰化 </p> <ul class="e_box p_dataSource e_box p_dataSource borderB_default" data-ename="資訊信息"> <li id="9vh9b8c" class="sort"><span id="b44jgdv" class="i_sort">分類(lèi)：</span><a href="/news/2/">行業(yè)新聞</a></li> <li id="xcjl8w4" class="auth"><span id="upgxovc" class="i_auth">作者：</span></li> <li id="344vceg" class="source"><span id="xse99ry" class="i_source">來(lái)源:</span></li>  <li id="gwdam9m" class="date"><span id="h8ryahe" class="i_pubDate">時(shí)間:</span>2020-10-20</li> <li id="c4mtkwy" class="view"><span id="oplsu9g" class="i_pvs">訪(fǎng)問(wèn)量：</span><span id="vfmoamo" class="p_viewCount">0</span></li> </ul>  </div>  <div id="qv9vctv" class="e_title p_articlesTitle" data-ename="描述標題"> <div id="rxo4nur" class="font">詳情 </div> </div> <div id="ozgnpwo" class="e_box p_articles" data-ename="資訊詳細描述"><div id="dikrtas" class='reset_style js-reset_style js-adapMobile '><p> 　　專(zhuān)利名稱(chēng)：偶氮二異庚腈生產(chǎn)工藝改進(jìn)的制作方法</p> <p> 　　技術(shù)領(lǐng)域：<span style="font-size: 12pt;">本發(fā)明屬于偶氮化合物生產(chǎn)工藝。</span></p> <p> 　　偶氮二異庚腈〔又名2·2′-偶氮(2·4-二甲基戊腈)〕是一種常用的高分子聚合引發(fā)劑。它的引發(fā)效率高，反應平穩，聚合產(chǎn)物質(zhì)量?jì)?yōu)，在聚氯乙烯生產(chǎn)中的應用尤為普遍。目前生產(chǎn)偶氮二異庚腈的工藝路線(xiàn)有二種一種是由甲基異丁基甲酮與肼反應生成己酮連氮，用氰氫酸氰化為二異庚腈肼，再用氯氣氧化為偶氮二異庚腈，該工藝氰化難，生產(chǎn)過(guò)程中易發(fā)生中毒事故;另一種是用次氯酸鈉氧化偶合2-氨基-2·4-二甲基戊腈(氨基庚腈)為2·2′-偶氮(2，4-二甲基戊腈)。日本山下和彥(JP57-56468)采用在與水互溶的有機溶劑中氧化，成本高，投資大。MOORE，E-ARL〔EP34437〕用十六烷基三甲基氯化銨相轉移催化劑等，在水相中氧化，但是該工藝不適用于低含量氨基庚腈，在加料過(guò)程中，先生成的產(chǎn)品逐步分解，產(chǎn)率很低。要將低濃度的氨基庚腈通過(guò)精餾來(lái)提濃是相當困難的，因為氨基庚腈在50℃以上就急劇分解，在11.5mmHg時(shí)氨基庚腈的沸點(diǎn)為77～79℃。在工藝生產(chǎn)中進(jìn)行10mmHg以下的真空蒸餾是難以實(shí)現的。因此，為何改進(jìn)已有的偶氮二異庚腈的生產(chǎn)工藝是一個(gè)重要課題。</p> <p> 　　本發(fā)明的目的是提供一種改進(jìn)的偶氮二異庚腈的生產(chǎn)工藝，該工藝操作簡(jiǎn)便、安全，投資少，成本低。</p> <p> 　　為達到上述目的，本發(fā)明采用以下工藝采用次氯酸鈉水溶液(有效氯含量為7～15%之間，游離堿含量為20～50g/l)來(lái)氧化偶合氨基庚腈，氨基庚腈的濃度在60～80%之間，氨基庚腈與次氯酸鈉的用量比為1∶1.5～1∶2.5(克分子比)。反應以三種季銨鹽表面活性劑配合一起作為相轉移催化劑，其中有一種為兩性表面活性劑，還加有促進(jìn)偶氮二異庚腈結晶增長(cháng)的溴化物，表面活性劑用量為氨基庚腈用量的1.0～2.0%(重量百分)，溴化物用量以溴離子的當量與表面活性劑的當量比，比例為1∶1～2∶1，反應在惰性氣體保護下，將氨基庚腈滴加到混合有表面活性劑和溴化物的次氯酸鈉溶液中，采用惰性氣體保護，可防止產(chǎn)物分解。反應溫度控制在5～10℃之間，滴加后再反應1小時(shí)，待漂浮顆粒變大后直接過(guò)濾，不必調節PH值，過(guò)濾后濾餅經(jīng)清洗、干燥，得到偶氮二異庚腈粗品，粗品可通過(guò)重結晶來(lái)提純。</p> <p> 　　上述談到的以三種季銨鹽表面活性劑配合一起作為相轉移催化劑使用，其中一種為兩性表面活性劑，其他二種可以是以通式</p> <p> 　　表示的季銨鹽，其中R1=C12～18，R2=C4～8R3、R4=C1～2，從價(jià)格、效果考慮，相轉移催化劑最好采用十八烷基三甲基氯化銨和十二烷基芐基二甲基氯化銨，甜菜堿配合一起使用。三種配合一起使用，偶氮二異庚腈的產(chǎn)率可提高至90%，各季銨鹽表面活性劑之間的用量比可采用1∶1(重量比)，也可以不等，在總用量范圍內作適當調整。</p> <p> 　　次氯酸鈉水溶液中，有效氯和游離堿的含量最好分別控制在12%和30g/l。在一般情況下反應中采用氮氣來(lái)保護。</p> <p> 　　本發(fā)明所提供的偶氮二異庚腈生產(chǎn)工藝，特別適用于低濃度的氨基庚腈生產(chǎn)偶氮二異庚腈。由于采用了三種季銨鹽表面活性劑作為相轉移催化劑以及惰性氣體保護，減少了分解產(chǎn)物的產(chǎn)生(分解產(chǎn)物為黃色油狀液體)，提高產(chǎn)率至90%，可以不考慮氨基庚腈的真空精餾提濃問(wèn)題，設備投資少，成本低。</p> <p> 　　以下結合實(shí)施例對本發(fā)明作進(jìn)一步說(shuō)明實(shí)施例1在1000ml三頸燒瓶中，加入570ml次氯酸鈉水溶液、(有效氯含量為12%，游離堿為30g/l)0.5g溴化鈉和1g十八烷基三甲基氯化銨，攪拌分散1小時(shí)后，滴加100ml2-氨基-2·4-二甲基戊腈(含量為70%)，滴加反應過(guò)程中，用氮氣保護，防止產(chǎn)物分解，溫度控制在5～10℃范圍內。滴加完畢后，再反應1小時(shí)，反應物由乳狀液逐漸澄清，漂浮顆粒變大為止。再經(jīng)過(guò)濾、水洗、低溫干燥得到偶氮二異庚腈42.3g，產(chǎn)率為70%。</p> <p> 　　實(shí)施例2相轉移催化劑用十二烷基芐基二甲基氯化銨代替十八烷基三甲基氯化銨，其他反應條件與實(shí)施例1相同。得偶氮二異庚腈41g，產(chǎn)率為68%。</p> <p> 　　實(shí)施例3相轉移催化劑用兩性的甜菜堿代替十八烷基三甲基氯化銨，其他反應條件與實(shí)施例1相同，得偶氮二異庚腈45.3g，產(chǎn)率為75%。</p> <p> 　　實(shí)施例4用兩種相轉移催化劑，十八烷基三甲基氯化銨和十二烷基芐基二甲基氯化銨各0.5g，代替十八烷基三甲基氯化銨，其他反應條件與實(shí)施例1相同，得偶氮二異庚腈50g，產(chǎn)率為83%。</p> <p> 　　實(shí)施例5用兩種相轉移催化劑，十八烷基三甲基氯化銨和甜菜堿各0.5g代替十八烷基三甲基氯化銨，其他反應條件與實(shí)施例1相同，得偶氮二異庚腈52.5g，產(chǎn)率為87%。</p> <p> 　　實(shí)施例6用兩種相轉移催化劑，十二烷基芐基二甲基氯化銨和甜菜堿各0.5g代替十八烷基三甲基氯化銨，其他反應條件與實(shí)施例1相同，得偶氮二異庚腈49.5g，產(chǎn)率為82%。</p> <p> 　　實(shí)施例7用三種相轉移催化劑，十八烷基三甲基氯化銨，十二烷基芐基二甲基氯化銨和甜菜堿各0.3g，代替十八烷基三甲基氯化銨，其他反應應條件與實(shí)施例1相同，得偶氮二異庚腈54.4g，產(chǎn)率為90%。</p> <p> 　　權利要求</p> <p> 　　1.一種制取偶氮二異庚腈工藝，它采用次氯酸鈉水溶液氧化偶合氨基庚腈來(lái)生成偶氮二異庚腈，其特征在于所采用的氨基庚腈的濃度在60～80%之間;反應以三種季銨鹽表面活性劑配合一起作相轉移催化劑，其中一種為兩性表面活性劑，其余二種是以通式表示的任意二種，通式</p> <p> 　　其中，R1=C12～18，R2=C4～8，R3、R4=C1～2;反應在惰性氣體保護下進(jìn)行。</p> <p> 　　2.按權利要求1所述的工藝，其特征在于所述的惰性氣體為氮氣，所述的相轉移催化劑為十八烷基三甲基氯化銨，十二烷基芐基二甲基氯化銨和甜菜堿三種配合一起使用。</p> </div></div>  <div id="xszbipc" class="e_box p_QRCode borderT_default" data-ename="打開(kāi)手機查看"> <p class="e_title p_SaveText" data-ename="二維碼引導信息"><span id="p4eld8w" class="i_qrcode">掃二維碼用手機看</span></p> <p class="e_image js_qrcode" data-ename="二維碼"></p> </div>  <div id="hct8seg" class="e_box d_pcDom p_PrevAndNext borderB_default" data-ename="上一篇、下一篇信息區"> <div id="bbnpby8" class="e_box p_previewBox"> <span id="gg8icj4" class="i_title"><span id="nn34dkw" class="i_pageUpTitle">上一個(gè)</span><span id="d3d3ov9" class="clons">:</span></span> <a href="/news/3.html" data-ename="上一篇信息區"> <span id="ine9iph" class="p_PreviewTitle">偶氮二異戊腈和偶氮二異丁腈的區別</span> </a> </div>  <div id="kaholxp" class="e_box p_nextBox"> <span 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"您輸入的驗證碼有誤，或已失效。", correct: " 請輸入正確的", correctG: " 請輸入正確格式的", hm: " 號碼", id: "portalResMessage_form-15822706865037602", lib: ["js/portalMessage/portalResMessage_form-01"], noDataFlag: "", success: "提交成功", submitRepeat: " 1分鐘內無(wú)法重復提交", submitError: " 暫時(shí)無(wú)法正常提交，請您稍后再試", submitUrl: "", submitTarget: "", selectId: "1", }) </script> </div></div> </div> </div></div><div class="39sovxe" id="w_fline-1584612322390" class="w_fline-001"><div id="t9yk4r9" class="w_fline"> <div id="tz4bifs" class="e_line e_Hline-001 p_FLine"></div> </div></div><div class="8eqx9n4" id="w_grid-1584612364244" class="w_grid-001"><div id="alx4rdf" class="w_grid signal"> <div id="hszbda4" class="e_box e_box-000 p_gridbox"> <div class="wmo9d8g" id="content_box-1584612364244-0" class="e_box e_box-000 d_gridCell_0 p_gridCell"><div class="ms9np3n" id="w_common_text-1584612356288" class="reset_style"><div><p><span style="font-size:14px"><span style="line-height:1.8"><span style="color:#a7c1dd"><span 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