CN114315789A - 一种l-丙交酯的制备方法 - Google Patents
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- JJTUDXZGHPGLLC-IMJSIDKUSA-N 4511-42-6 Chemical compound C[C@@H]1OC(=O)[C@H](C)OC1=O JJTUDXZGHPGLLC-IMJSIDKUSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 150000003839 salts Chemical class 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical compound CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 13
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 claims abstract description 10
- 150000008301 phosphite esters Chemical class 0.000 claims abstract description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 36
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 235000014655 lactic acid Nutrition 0.000 claims description 18
- 239000004310 lactic acid Substances 0.000 claims description 18
- 238000005336 cracking Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 8
- 238000006116 polymerization reaction Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000010408 film Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims description 5
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 5
- 239000004626 polylactic acid Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 3
- QQBLOZGVRHAYGT-UHFFFAOYSA-N tris-decyl phosphite Chemical compound CCCCCCCCCCOP(OCCCCCCCCCC)OCCCCCCCCCC QQBLOZGVRHAYGT-UHFFFAOYSA-N 0.000 claims description 3
- OQBLGYCUQGDOOR-UHFFFAOYSA-L 1,3,2$l^{2}-dioxastannolane-4,5-dione Chemical compound O=C1O[Sn]OC1=O OQBLGYCUQGDOOR-UHFFFAOYSA-L 0.000 claims description 2
- NOWFQOWNIXZVPF-UHFFFAOYSA-N C(CCCCCCC(C)C)OP(OCCCCCCCC(C)C)OP(O)O.C(O)C(CO)(CO)CO Chemical compound C(CCCCCCC(C)C)OP(OCCCCCCCC(C)C)OP(O)O.C(O)C(CO)(CO)CO NOWFQOWNIXZVPF-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- KUMNEOGIHFCNQW-UHFFFAOYSA-N diphenyl phosphite Chemical compound C=1C=CC=CC=1OP([O-])OC1=CC=CC=C1 KUMNEOGIHFCNQW-UHFFFAOYSA-N 0.000 claims description 2
- 239000011552 falling film Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- FSBZGYYPMXSIEE-UHFFFAOYSA-H tin(2+);diphosphate Chemical compound [Sn+2].[Sn+2].[Sn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O FSBZGYYPMXSIEE-UHFFFAOYSA-H 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- JJTUDXZGHPGLLC-ZXZARUISSA-N (3r,6s)-3,6-dimethyl-1,4-dioxane-2,5-dione Chemical compound C[C@H]1OC(=O)[C@H](C)OC1=O JJTUDXZGHPGLLC-ZXZARUISSA-N 0.000 abstract description 11
- 150000002500 ions Chemical class 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- -1 stannum ions Chemical class 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 238000012691 depolymerization reaction Methods 0.000 abstract 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 4
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 150000001339 alkali metal compounds Chemical class 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000006340 racemization Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1845—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing phosphorus
- B01J31/185—Phosphites ((RO)3P), their isomeric phosphonates (R(RO)2P=O) and RO-substitution derivatives thereof
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
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- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
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- B01J31/22—Organic complexes
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- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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Abstract
本发明公开了一种L‑丙交酯的制备方法，本发明以L‑乳酸为原料，在催化剂的催化作用下制备得到L‑丙交酯；所述催化剂是由亚锡盐和亚磷酸酯在溶剂中反应得到，其可以有效的抑制二价的亚锡离子氧化成四价的锡离子；有效降低内消旋丙交酯的转化率；提升L‑丙交酯的产率；并获得接近白色的L‑丙交酯。在解聚反应过后生成的粗丙交酯中，L‑丙交酯的含量≥95％；内消旋丙交酯含量≤3.8％，同时保证残液的颜色接近乳白色。
Description
本申请是申请日为2020年12月15日、申请号为202011480932.2、发明名称为《一种亚锡盐配合物催化剂及其生产L-丙交酯的方法》的发明专利的分案申请。
技术领域
本发明属于L-丙交酯制备技术领域，具体涉及一种L-丙交酯的制备方法。
背景技术
目前制备丙交酯常用的裂解催化剂主要为锌、锡等金属及其金属盐，其中应用范围最广的主要是亚锡盐，包括辛酸亚锡、氯化亚锡、硫酸亚锡等。但是，亚锡盐极易被氧化，特别是在裂解反应条件下(＞200℃)，快速氧化分解，生成四价锡盐，从而失去催化活性，而锡盐还会导致丙交酯的消旋，使得生成内消旋丙交酯的量增加。同时，还会造成丙交酯和残液的颜色加深。
CN101903370B公开了亚磷酸亚锡作为合成丙交酯的裂解催化剂。采用亚磷酸的还原性阻止了亚锡离子氧化成锡离子，从而降低内消旋丙交酯的转化率，并改善了丙交酯的色相。但亚磷酸盐的毒性较大，可在酸性条件下生成剧毒的磷化氢，安全性较差。CN110156745A公开了一种锌类化合物和/或锡类化合物与碱金属化合物的复合催化剂，但碱金属化合物的加入并不能改善亚锡盐被氧化成锡盐。GB 2331986A公开了辛酸亚锡与亚磷酸酯稳定剂复配使用，用于制备丙交酯。但亚磷酸酯仅作为稳定剂，并没有与亚锡盐进行配位反应，并不能完全阻止亚锡盐被氧化成锡盐，并且只是提升的丙交酯的色相，并未降低内消旋丙交酯的转化率。
发明内容
本发明的目的在于：提供一种L-丙交酯的制备方法，本发明以L-乳酸为原料在催化剂的作用下制备得到L-丙交酯，本发明提供的催化剂制备过程简单无污染、对设备要求低、便于工业化，催化剂在高温下稳定性高，亚锡盐不会被氧化成四价的锡盐，且本发明得到的L-丙交酯色相好、内消旋丙交酯含量小、残液的色相好。
为达到上述目的，本发明采取了如下技术方案：
一种L-丙交酯的制备方法，包括如下制备步骤：
(1)将质量浓度为80～98％的L-乳酸水溶液连续加入到带有精馏装置的第一反应釜中，在温度80～120℃，真空度-0.05～-0.09MPa下，脱出游离水和结合水，反应产生的水、乳酸蒸汽经精馏塔分离，塔顶水蒸气经冷凝后流入收集罐中，控制低聚乳酸聚合度为2～8，将低聚乳酸通过泵连续输送到第二反应釜中；
(2)第二反应釜也带有精馏装置，低聚乳酸在温度120～170℃，真空度-0.1MPa下，进一步聚合，控制低聚乳酸的聚合度为8～25，将低聚乳酸与连续注入的亚锡盐配合物催化剂，通过泵连续输送至静态混合器混合均匀后，输送到第三反应器中；
(3)低聚乳酸在第三反应器中进行裂解反应，反应温度为200～230℃，压力为50～500Pa，低聚乳酸裂解生成的粗丙交酯蒸汽经冷凝收集在粗交酯储罐中，同时未蒸发的残夜流入残液收集罐中；对粗丙交酯进行提纯，得到达到熔融聚合反应所需纯度的L-丙交酯；
所述亚锡盐配合物催化剂的制备步骤如下：
(1)将亚锡盐溶于溶剂中，加热回流30min，使亚锡盐充分溶解；
(2)在氮气保护下，将亚磷酸酯滴加至亚锡盐溶液中，并回流反应2h，亚锡盐与亚磷酸酯的质量比为5：1～20：1，亚锡盐与溶剂的质量比为2：1～1：5；
(3)反应结束后，将溶剂从体系中抽出并回收再利用，最终生成的淡黄色粘稠液体即为亚锡盐配合物催化剂成品。
优选的，所述亚锡盐为异辛酸亚锡、氯化亚锡、硫酸亚锡、草酸亚锡、磷酸亚锡中的一种或两种及以上组成。
优选的，所述亚磷酸酯为亚磷酸三苯酯、亚磷酸三癸酯、亚磷酸二苯酯、二亚磷酸季戊四醇二异癸酯中的一种或两种及以上组成。
优选的，所述溶剂为苯、甲苯、乙酸乙酯、丙酮、二甲苯中的一种或两种及以上组成。
优选的，所述亚锡盐配合物催化剂的加入量为低聚物质量的0.5～5％。
优选的，所述第三反应器为笼式蒸发反应器、刮板式薄膜蒸发器、降膜式蒸发器、升膜式蒸发器中的一种。
优选的，所述粗丙交酯可通过本技术领域人员已知提纯技术，如熔融结晶、精馏、溶剂重结晶等方式进行提纯。
优选的，所述步骤(3)中产生的残液回用至所述步骤(2)中和低聚乳酸、亚锡盐配合物催化剂进行混合。
本发明的有益效果：本发明通过利用亚锡盐与亚磷酸酯的配位反应制备催化剂，能够显著地提高催化剂在高温下的稳定性，可以有效的抑制二价的亚锡离子氧化成四价的锡离子；有效降低内消旋丙交酯的转化率，提升L-丙交酯的产率，并获得接近白色的L-丙交酯，在解聚反应过后生成的粗丙交酯中，L-丙交酯的含量≥95％；内消旋丙交酯含量≤3.8％，同时保证残液的颜色接近乳白色。
具体实施方式
下面结合具体实施例对本发明做进一步说明，但本发明不仅仅限定于这些实施例。
实施例
1.亚锡盐配合物催化剂的制备：
将100g异辛酸亚锡加入50g甲苯中，110℃下，回流溶解30min，将20g亚磷酸三癸酯加入到异辛酸亚锡和甲苯的混合溶液中，继续回流反应2h，反应结束后，在真空下抽出反应体系中的甲苯，并回收再利用，最后得到的淡黄色粘稠液体即为亚锡盐配合物催化剂。
2.低聚乳酸的制备：
将质量浓度为90％的L-乳酸水溶液以15kg/h的速率加入到第一反应釜中，第一反应釜带有精馏塔，反应温度恒定为120℃，真空度为-0.08MPa，停留时间为2h，控制低聚乳酸聚合度为6～8，将反应产物低聚乳酸用泵连续输送到第二反应釜中。
第二反应釜也带有精馏装置，低聚乳酸在温度160℃，真空度-0.1MPa下，进一步聚合，控制低聚乳酸的聚合度为15～20，反应产物低聚乳酸用泵连续输送到第三反应器中。
3.低聚乳酸裂解生成粗丙交酯：
来自第二反应釜的低聚乳酸与连续注入的亚锡盐配合物催化剂经静态混合器混合后，以13kg/h的速率加入到蒸发面积为0.8m2的升膜式蒸发器中，其中亚锡盐配合物催化剂的使用量为低聚乳酸质量的1％，蒸发器反应温度为230℃，并控制压力为500Pa，粗丙交酯不断产生，并冷凝收集在丙交酯储罐中，同时未蒸发的残液流入残液收集罐中，所述粗丙交酯的组分如表1所示。
4.残液的循环使用：
将裂解产生的残液采用连续注入的方式与低聚乳酸、亚锡盐配合物催化剂经静态混合器混合后，重新加入到升膜式蒸发器中，循环运行一个月后，粗丙交酯的组分如表2所示。
对比例
对比例使用的催化剂为异辛酸亚锡，其用量及用于生产丙交酯的方法与实施例相同。
表1残液未循环使用时得到的粗丙交酯的组成
| 粗丙交酯的组成(重量％) | 实施例 | 对比例 |
| L-丙交酯 | 94.7 | 87.8 |
| 内消旋丙交酯 | 3.1 | 10.0 |
| 乳酸 | 0.7 | 0.7 |
| 乳酸低聚物 | 1.0 | 1.1 |
| 粗丙交酯的颜色 | 白色 | 微黄色 |
| 产率％(L-丙交酯/低聚乳酸) | 88.26 | 80.96 |
| 残液的颜色 | 白色浑浊 | 褐色浑浊 |
表2残液循环使用后得到的粗丙交酯的组成
从表1中可以看出，使用亚锡盐配合物催化剂后，L-丙交酯的纯度有明显的提升，同时内消旋丙交酯明显降低，粗丙交酯及残液的颜色均较好。从表2中可以看出，在残液全部回收循环使用运行一个月之后，实施例中的L-丙交酯纯度有一定程度降低，但对比例中L-丙交酯纯度降低更为明显，且粗丙交酯的颜色较深，残液的颜色变为褐色。由此可见，本发明技术提供的亚锡盐催化剂生产丙交酯能够增加L-丙交酯的纯度，降低内消旋丙交酯的生成量，提升丙交酯及残液的颜色。
上述实施例仅例示出本公开的具体实施方案，但是本公开的实施方案并不受上述内容的限制。在未实质性背离本公开的发明构思的主旨和原理的情况下所做出的任何改变、修饰、替代、组合、简化，均应为等效的置换方式，并包含在由权利要求所确定的保护范围之内。
Claims (8)
1.一种L-丙交酯的制备方法，其特征在于：包括如下制备步骤：
(1)将质量浓度为80～98％的L-乳酸水溶液连续加入到带有精馏装置的第一反应釜中，在温度80～120℃，真空度-0.05～-0.09MPa下，脱出游离水和结合水，反应产生的水、乳酸蒸汽经精馏塔分离，塔顶水蒸气经冷凝后流入收集罐中，控制低聚乳酸聚合度为2～8，将低聚乳酸通过泵连续输送到第二反应釜中；
(2)第二反应釜也带有精馏装置，低聚乳酸在温度120～170℃，真空度-0.1MPa下，进一步聚合，控制低聚乳酸的聚合度为8～25，将低聚乳酸与连续注入的亚锡盐配合物催化剂，通过泵连续输送至静态混合器混合均匀后，输送到第三反应器中；
(3)低聚乳酸在第三反应器中进行裂解反应，反应温度为200～230℃，压力为50～500Pa，低聚乳酸裂解生成的粗丙交酯蒸汽经冷凝收集在粗交酯储罐中，同时未蒸发的残液流入残液收集罐中；对粗丙交酯进行提纯，得到达到熔融聚合反应所需纯度的L-丙交酯；
所述亚锡盐配合物催化剂的制备步骤如下：
(1)将亚锡盐溶于溶剂中，加热回流30min，使亚锡盐充分溶解；
(2)在氮气保护下，将亚磷酸酯滴加至亚锡盐溶液中，并回流反应2h，亚锡盐与亚磷酸酯的质量比为5：1～20：1，亚锡盐与溶剂的质量比为2：1～1：5；
(3)反应结束后，将溶剂从体系中抽出并回收再利用，最终生成的淡黄色粘稠液体即为亚锡盐配合物催化剂成品。
2.如权利要求1所述的制备方法，其特征在于：所述亚锡盐为异辛酸亚锡、氯化亚锡、硫酸亚锡、草酸亚锡、磷酸亚锡中的一种或两种及以上组成。
3.如权利要求1所述的制备方法，其特征在于：所述亚磷酸酯为亚磷酸三苯酯、亚磷酸三癸酯、亚磷酸二苯酯、二亚磷酸季戊四醇二异癸酯中的一种或两种及以上组成。
4.如权利要求1所述的制备方法，其特征在于：所述溶剂为苯、甲苯、乙酸乙酯、丙酮、二甲苯中的一种或两种及以上组成。
5.如权利要求1所述的制备方法，其特征在于：所述亚锡盐配合物催化剂的加入量为低聚物质量的0.5～5％。
6.如权利要求1所述的制备方法，其特征在于：所述第三反应器为笼式蒸发反应器、刮板式薄膜蒸发器、降膜式蒸发器、升膜式蒸发器中的一种。
7.如权利要求1所述的制备方法，其特征在于：所述粗丙交酯通过熔融结晶、精馏、溶剂重结晶中的一种方式或几种方式进行提纯。
8.如权利要求1所述的制备方法，其特征在于，所述步骤(3)中产生的残液回用至所述步骤(2)中和低聚乳酸、亚锡盐配合物催化剂进行混合。
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