(一) 製品的凍結
溶液速凍時(每分鍾降溫10~50℃),晶粒保持在顯微鏡下可見的大小;相反慢凍時(1℃/分),形xing成cheng的de結jie晶jing肉rou眼yan可ke見jian。粗cu晶jing在zai升sheng華hua留liu下xia較jiao大da的de空kong隙xi,可ke以yi提ti高gao凍dong幹gan的de效xiao率lv,細xi晶jing在zai升sheng華hua後hou留liu下xia的de間jian隙xi較jiao小xiao,使shi下xia層ceng升sheng華hua受shou阻zu,速su成cheng凍dong的de成cheng品pin粒li子zi細xi膩ni,外wai觀guan均jun勻yun,比bi表biao麵mian積ji大da,多duo孔kong結jie構gou好hao,溶rong解jie速su度du快kuai,便bian成cheng品pin的de引yin濕shi性xing相xiang對dui也ye要yao強qiang些xie。
藥品在凍幹機中預凍在兩種方式:一種是製品與幹燥箱同時降溫,;另一種是待幹燥箱擱板降溫至-40℃zuoyou,zaijiangzhipinfangru,qianzhexiangdangyumandong,houzhezejieyudongyumandongzhijian,yinerchangbeicaiyong,yijiangudongganxiaolvyuchanpinzhiliang。cifadequedianshizhipinruxiangshi,kongqizhongdeshuizhengqijiangxunsudiningjiezaigebanshang,erzaishenghuachuqi,ruobanshengwenjiaokuai,youyudamianjideshenghuajiangyoukenengchaoyueningjieqidezhengchangfuhe。cixianxiangzaixiajiyouweixianzhu。
zhipindedongjiechuyujingzhizhuangtai。jingyanzhengming,guolengxianxiangrongyifashengzhishizhipinwendusuiyidadaogongjingdian。danrongzhirengbujiejing,weilekefuguolengxianxiang,zhipindongjiedewenduyingdiyugongjingdianyixiayigefanwei,bingxubaochiyiduanshijian,yidaizhipinwanquandongjie。
(二) 升華的條件與速度
冰在一定溫度下的飽和蒸汽壓大於環境的水蒸氣分壓時即可開始升華;比製品溫更低的凝結器對水水蒸氣的抽吸與捕獲作用,則是維護升所必需的條件。
qitifenzizailiangcilianxupengzhuangzhijiansuozoudejulichengweipingjunziyoucheng,tayuyalichengfanbi。zaichangyaxia,qizhihenxiao,shenghuadeshuifenzihenrongyiyuqitipengzhuangyoufanhuidaozhengqiyuanbiaomian,yinershenghuasuduhenman。suizheyalijiangdi13.3Pa以下,平均自由程增大105倍,使升華速度顯著加快,飛離出來的水分子很少改變自己的方麵,從而形成了定向的蒸汽流。
真空泵在凍幹機中起著抽除永久氣體的作用,以維護升華所必需的低壓強。1g水蒸氣在常壓下為1.25L而在13.3Pa時卻膨脹為10000升,普通的真空泵在單位時間內抽除如此大量的體積是不可能的。凝結器實際上形成了專門捕集水蒸氣的真空泵。
製品與凝結的溫度通常為-25℃與-50℃。冰在該溫度下的飽和蒸汽壓分別為63.3Pa與1.1Pa,因而在升華麵與冷凝麵之間便產生了一個相當大的壓力差,如果此時係統內的不凝性氣體分壓可以忽略不計,它將促使製品升華出來的水蒸氣,以一定的流速定向地抵達凝結器表麵結成冰霜。
冰的升華熱約為2822J/ke,ruguoshenghuaguochengbugonggeireliang,namozhipinzhiyoujiangdineinenglaibuchangshenghuare,zhizhiqiwenduyuningjieqiwendupinghenghou,shenghuayejiutingzhile。weilebaochishenghuayulengninglaidewenducha,bixuduizhipintigongzugoudereliang。
(2)升華過程
在升溫的第一階段(大量升華階段),製(zhi)品(pin)溫(wen)度(du)要(yao)低(di)於(yu)其(qi)共(gong)晶(jing)點(dian)一(yi)個(ge)範(fan)圍(wei)。因(yin)此(ci)擱(ge)板(ban)溫(wen)要(yao)加(jia)以(yi)控(kong)製(zhi),若(ruo)製(zhi)品(pin)已(yi)經(jing)部(bu)分(fen)幹(gan)燥(zao),但(dan)溫(wen)度(du)卻(que)超(chao)過(guo)了(le)其(qi)共(gong)晶(jing)點(dian),此(ci)時(shi)將(jiang)發(fa)生(sheng)製(zhi)品(pin)融(rong)化(hua)現(xian)象(xiang),而(er)此(ci)時(shi)融(rong)化(hua)的(de)液(ye)體(ti),對(dui)冰(bing)飽(bao)和(he),對(dui)溶(rong)質(zhi)卻(que)未(wei)飽(bao)和(he),因(yin)而(er)幹(gan)燥(zao)的(de)溶(rong)質(zhi)將(jiang)迅(xun)速(su)溶(rong)解(jie)進(jin)去(qu),最(zui)後(hou)濃(nong)縮(suo)成(cheng)一(yi)薄(bo)僵(jiang)塊(kuai),外(wai)觀(guan)極(ji)為(wei)不(bu)良(liang),溶(rong)解(jie)速(su)度(du)很(hen)差(cha),若(ruo)製(zhi)品(pin)的(de)融(rong)化(hua)發(fa)生(sheng)在(zai)大(da)量(liang)升(sheng)華(hua)後(hou)期(qi),則(ze)由(you)於(yu)融(rong)化(hua)的(de)液(ye)體(ti)數(shu)量(liang)較(jiao)少(shao),因(yin)而(er)被(bei)幹(gan)燥(zao)的(de)孔(kong)性(xing)固(gu)體(ti)所(suo)吸(xi)收(shou),造(zao)成(cheng)凍(dong)幹(gan)後(hou)塊(kuai)狀(zhuang)物(wu)有(you)所(suo)缺(que)損(sun),加(jia)水(shui)溶(rong)解(jie)時(shi)仍(reng)能(neng)發(fa)現(xian)溶(rong)解(jie)速(su)度(du)較(jiao)慢(man)。
在大量升華過程,雖然擱板和製品溫度有很大懸殊,但由於板溫、凝(ning)結(jie)器(qi)溫(wen)度(du)和(he)真(zhen)空(kong)溫(wen)度(du)基(ji)本(ben)不(bu)變(bian),因(yin)而(er)升(sheng)華(hua)吸(xi)熱(re)比(bi)較(jiao)穩(wen)定(ding),製(zhi)品(pin)溫(wen)度(du)相(xiang)對(dui)恒(heng)定(ding)。隨(sui)著(zhe)製(zhi)品(pin)自(zi)上(shang)而(er)下(xia)層(ceng)層(ceng)幹(gan)燥(zao),冰(bing)層(ceng)升(sheng)華(hua)的(de)阻(zu)力(li)逐(zhu)漸(jian)增(zeng)大(da)。製(zhi)品(pin)溫(wen)度(du)相(xiang)應(ying)也(ye)會(hui)小(xiao)幅(fu)上(shang)升(sheng)。直(zhi)至(zhi)用(yong)肉(rou)眼(yan)已(yi)不(bu)到(dao)冰(bing)晶(jing)的(de)存(cun)在(zai)。此(ci)時(shi)90%以yi上shang的de水shui分fen已yi除chu去qu。大da量liang升sheng華hua的de過guo程cheng至zhi此ci已yi基ji本ben結jie束shu,為wei了le確que保bao整zheng箱xiang製zhi品pin大da量liang升sheng華hua完wan畢bi,板ban溫wen仍reng需xu保bao持chi一yi個ge階jie段duan後hou再zai進jin行xing第di二er階jie段duan的de升sheng溫wen。
shengyubaifenzhijideshuifenchengcanyushuifen,tayuziyouzhuangtaideshuizaiwulihuaxuexingzhishangyousuobutong,canyushuifenbaokuolehuaxuejiehezhishuiyuwulijiehezhishui,zhuruhuahedejiejingshuijiejing、danbaizhitongguoqingjianjiehedeshuiyijigutibiaomianhuomaoxiguanzhongxifushuideng。youyucanyushuifenshoudaozhongyinlideshufu,qibaohezhengqiyazeshibutongchengdudejiangdi,yinerganzaosudumingxianxiajiang。suirantigaozhipinwenducujincanyushuifendeqihua,danruochaoguomoujixianwendu,shengwuhuoxingyekenengjijuxiajiang。baozhengzhipinanquandezuigaoganzaowenduyaoyoushiyanlaiqueding。tongchangwomenzaidierjieduanjiangbanwen+30℃左zuo右you,並bing保bao持chi恒heng定ding。在zai這zhe一yi階jie段duan初chu期qi,由you於yu板ban溫wen升sheng高gao,殘can餘yu水shui分fen少shao又you不bu易yi氣qi化hua,因yin此ci製zhi品pin溫wen度du上shang升sheng較jiao快kuai。但dan隨sui著zhe製zhi品pin溫wen度du與yu板ban溫wen逐zhu漸jian靠kao攏long,熱re傳chuan導dao變bian得de更geng為wei緩huan慢man,需xu要yao耐nai心xin等deng待dai相xiang當dang長chang的de一yi段duan時shi間jian,實shi踐jian經jing驗yan表biao明ming,殘can餘yu水shui分fen幹gan燥zao的de時shi間jian與yu大da量liang升sheng華hua的de時shi間jian幾ji乎hu相xiang等deng有you時shi甚shen至zhi還hai會hui超chao過guo。
(四)凍幹曲線:將擱板溫度與製品溫度隨時間的變化記錄下來,即可得到凍幹曲線。
比較典型的凍幹曲線係將擱板升溫分為兩個階段,在大量升華時擱板溫度保持較低,根據實際情況,一般可控製在-10至+10之zhi間jian。第di二er階jie段duan則ze根gen據ju製zhi品pin性xing質zhi將jiang擱ge板ban溫wen度du適shi當dang調tiao高gao,此ci法fa適shi用yong於yu其qi熔rong點dian較jiao低di的de製zhi品pin。若ruo對dui製zhi品pin的de性xing能neng尚shang不bu清qing楚chu,機ji器qi性xing能neng較jiao差cha或huo其qi工gong作zuo不bu夠gou穩wen定ding時shi,用yong此ci法fa也ye比bi較jiao穩wen妥tuo。
如(ru)果(guo)製(zhi)品(pin)共(gong)晶(jing)點(dian)較(jiao)高(gao),係(xi)統(tong)的(de)真(zhen)空(kong)度(du)也(ye)能(neng)保(bao)持(chi)良(liang)好(hao),凝(ning)結(jie)器(qi)的(de)製(zhi)冷(leng)能(neng)力(li)充(chong)裕(yu),則(ze)也(ye)可(ke)采(cai)用(yong)一(yi)定(ding)的(de)升(sheng)溫(wen)速(su)度(du),將(jiang)擱(ge)板(ban)溫(wen)度(du)升(sheng)高(gao)至(zhi)允(yun)許(xu)的(de)最(zui)高(gao)溫(wen)度(du),直(zhi)至(zhi)凍(dong)幹(gan)結(jie)束(shu),但(dan)也(ye)需(xu)保(bao)證(zheng)製(zhi)品(pin)在(zai)大(da)量(liang)升(sheng)華(hua)時(shi)的(de)溫(wen)度(du)不(bu)得(de)超(chao)過(guo)共(gong)晶(jing)點(dian)。
若製品對熱不穩定,則第二階段板溫不宜過高。為了提高第一階段的升華速度,可將拉板溫度一次升高至製品允許的最高溫度以上;待dai大da量liang升sheng華hua階jie段duan基ji本ben結jie束shu時shi,再zai將jiang板ban溫wen降jiang至zhi允yun許xu的de最zui高gao溫wen度du,這zhe後hou兩liang種zhong方fang式shi雖sui然ran使shi大da量liang的de升sheng華hua速su度du有you一yi些xie提ti高gao,但dan其qi抗kang幹gan擾rao的de能neng力li相xiang應ying降jiang低di,真zhen空kong度du和he製zhi冷leng能neng力li的de突tu然ran降jiang低di或huo停ting電dian都dou可ke能neng會hui使shi製zhi品pin融rong化hua。合he理li而er靈ling活huo地di掌zhang握wo第di一yi種zhong方fang式shi,仍reng是shi目mu前qian較jiao常chang用yong的de方fang式shi。
手機版




