真空冷冻干燥技术讲解⑶

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! O! W; ~4 ?/ [5 n$ _8 g( C" y                                                <P style="LINE-HEIGHT: 18pt; TEXT-ALIGN: center; mso-line-height-rule: exactly" align=center><B><SPAN style="FONT-SIZE: 16pt; COLOR: black"><FONT face=宋体>真空冷冻干燥技术讲解⑶<SPAN lang=EN-US><?xml:namespace prefix = o ns = "urn:schemas-microsoft-com:office:office" /><o:p></o:p></SPAN></FONT></SPAN></B></P>
- O, f0 D5 c- O6 T8 @0 T6 P<P class=MsoNormal style="MARGIN: 0cm 0cm 7&#46;8pt; TEXT-ALIGN: center; mso-para-margin-bottom: &#46;5gd" align=center><B><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">上海东富龙科技有限公司 张耀平<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></B></P>
, @+ Q, @) N# D, @+ j! j: }<P class=MsoNormal style="MARGIN: 0cm 0cm 7&#46;8pt; LINE-HEIGHT: 22pt; TEXT-ALIGN: center; mso-line-height-rule: exactly; mso-para-margin-bottom: &#46;5gd" align=center><B><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">第四节 冻干产品的崩解温度<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></B></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly; mso-char-indent-count: 2&#46;0"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">对于冻干产品的共熔点大家已经熟悉了，它就是产品的真正固化点。也就是产品在抽真空前必须冷却到的那个温度点，不然产品在抽空时将会起泡，在升华加热的时候也不能使产品超过这个温度，不然产品将熔化。因此，共熔点是在预冻阶段和升华阶段需要进行控制的温度值。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
9 z( [" i+ C7 c# v' g  i7 u( ~<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">现在引入一个崩解温度的概念，它是不同于共熔点的另外一个温度。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">一个正常升华的产品，当升华进行到一定的时候，就会出现上层的干燥层和下层的冻结层，这二层之间的交界面就是升华面，升华面是随着升华的进行而不断下降的。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
7 h0 H6 q; y- J% u# _$ g& |<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">已经干燥的产品应该是疏松多孔，并保持在这一稳定的状态，以便下层冻结产品升华出来的水蒸汽能顺利地通过，使全部产品都得到良好的干燥。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">但某些已经干燥的产品当温度升高到某一数值时，会失去刚性，变得有粘性，发生类似塌方的崩解现象，使干燥产品失去疏松多孔的状态，封闭了下层冻结产品水蒸汽的逸出通路，妨碍了升华的继续进行。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">于是，升华速率变慢，从冻结产品吸收升华热也随之减少，由板层供给的热量将有多余，这样便引起冻结产品的温度上升，当温度升高到共熔点以上的温度时，产品就会发生熔化或发泡现象，致使冻干失败。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
( I/ o# u2 S+ n- {' F: I1 |<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">发生崩解时的温度叫做该产品的崩解温度。对于这样的产品要获得良好的干燥，只有保持升华中的干燥产品的温度在崩解点以下，直到冻结产品全部升华完毕为止，才能使产品温度继续上升。这时由于产品中已不存在冻结冰，干燥产品即使发生崩解也不会影响产品的干燥，因为产品已从升华阶段转入解吸干燥阶段。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
! C- j4 n6 W5 n5 ~3 M& `<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">没有发生崩解的干燥产品与发生崩解的干燥产品在外观上用肉眼看不出有什么差别，只有在显微镜下才能看到结构上的变化。当在显微镜下观察产品的冷冻干燥过程时，如果看到发生崩解现象，那么这时的温度就是该产品的崩解温度。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">有些产品的崩解温度高于共熔点温度，那么升华时仅需控制产品温度低于共熔点温度就行了；但有些产品的崩解温度低于共熔点温度，那么按照一般的方法控制升华时就可能发生崩解现象，这样的产品只有在较低的温度下进行升华，因此必须延长冻干时间。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">产品的共熔点可以通过电阻法、差示热分析法和低温显微镜直接观察法得知，但产品的崩解温度只有在冷冻干燥显微镜下直接观察才能得知。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21&#46;75pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">产品的崩解温度取决于产品本身的品种和保护剂的种类；混合物质的崩解温度取决于各组分的崩解温度。因此在选择产品的冻干保护剂时，应选择具有较高崩解温度的材料，使升华干燥能在不很低的温度下进行，以节省冻干的能耗和时间，提高生产率。<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly; mso-char-indent-count: 2&#46;0"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">甘氨酸、甘露醇、葡聚糖、木糖醇、聚已烯吡咯烷酮和蛋白质混合物等保护剂能提高产品的崩解温度。一些物质的崩解温度℃见表二十三<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
! Z' K' N6 Y# A3 U2 W  F2 v<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN lang=EN-US style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt"><o:p> </o:p></SPAN></P>
% \6 R6 M$ A  z, y<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-INDENT: 21pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly; mso-char-indent-count: 2&#46;0"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">表二十三<SPAN lang=EN-US><SPAN style="mso-spacerun: yes">  </SPAN></SPAN>一些物质的崩解温度℃<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
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<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; TEXT-ALIGN: center; mso-line-height-rule: exactly" align=center><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">温度℃<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P></TD></TR>
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<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">葡聚糖（右旋糖苷）<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
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<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">聚蔗糖<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">果糖<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
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<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">葡萄<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">右旋葡萄糖<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
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<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">乳糖<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">马尼妥<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
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<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">枸椽酸<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">硫胺素硝酸盐<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">吡哆醇<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
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6 G( _" }$ c6 M- u3 J<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">抗坏血酸<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
* v& I/ s3 v4 I* {<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">纳·阿斯考派脱<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
. Q6 w: |5 Q  e/ n5 W/ `1 q$ I& [<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">烟酰胺<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
7 ]/ n5 U2 y# S9 V4 P$ _3 K# y<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">钙·潘妥颠<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
7 z  V* B3 Y& z2 c. F8 L. p; Z<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">乙酸胺<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">钠·巴比妥<SPAN lang=EN-US><o:p></o:p></SPAN></SPAN></P></TD>
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4 j1 j' ]) W  Y<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN lang=EN-US style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">10<o:p></o:p></SPAN></P>
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; N' v' }1 @7 G1 \4 u2 o5 k<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">－<SPAN lang=EN-US>27<o:p></o:p></SPAN></SPAN></P>
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<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">－<SPAN lang=EN-US>4<o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">－<SPAN lang=EN-US>37<o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">－<SPAN lang=EN-US>37<o:p></o:p></SPAN></SPAN></P>
0 a, [, p: _- c! U<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">－<SPAN lang=EN-US>33<o:p></o:p></SPAN></SPAN></P>
6 h% P. q9 y7 ^" e5 f' v5 d  {<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">－<SPAN lang=EN-US>4<o:p></o:p></SPAN></SPAN></P>
& g$ w1 I  j& e<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">－<SPAN lang=EN-US>19<o:p></o:p></SPAN></SPAN></P>
7 ]  a3 r' s5 f9 s! W<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">－<SPAN lang=EN-US>25<o:p></o:p></SPAN></SPAN></P>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; LINE-HEIGHT: 18pt; mso-line-height-rule: exactly"><SPAN style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt">－<SPAN lang=EN-US>4<o:p></o:p></SPAN></SPAN></P></TD></TR></TBODY></TABLE>
<P class=MsoNormal style="MARGIN: 0cm 0cm 0pt; TEXT-ALIGN: center" align=center><SPAN lang=EN-US style="COLOR: black; FONT-FAMILY: 宋体; mso-bidi-font-size: 10&#46;5pt"><o:p> </o:p></SPAN></P></td>
                               
                               
                                         
                                                </td>
8 ?% }7 U, v) T# _8 h7 V                               
                        </table>
                        <table cellSpacing="0" cellPadding="0" width="98%" align="center" border="0">