CN113373190B - Method for preparing galactomannan from semen Trigonellae - Google Patents

Method for preparing galactomannan from semen Trigonellae Download PDF

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CN113373190B
CN113373190B CN202110582035.0A CN202110582035A CN113373190B CN 113373190 B CN113373190 B CN 113373190B CN 202110582035 A CN202110582035 A CN 202110582035A CN 113373190 B CN113373190 B CN 113373190B
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CN113373190A (en
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张伟
曹毅
武建
刘燕静
袁江宏
袁润
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Chengde Kangerrun Biotechnology Co.,Ltd.
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Abstract

The invention discloses a method for preparing galactomannan from fenugreek. The method comprises the steps of firstly peeling fenugreek and lima beans, then adding water for tempering, mixing and crushing; then sanding the mixture in a sanding machine; adding water, mixing well to obtain water solution, adding mannase and galactosidase, and hydrolyzing to obtain enzymatic hydrolysate; finally, inactivating the enzymolysis liquid, cooling to room temperature, filtering, decolorizing, concentrating to obtain syrup, and vacuum drying to obtain galactomannan. The invention adopts fenugreek and lima beans as extraction raw materials to prepare the galactomannan, compared with the galactomannan obtained by singly adopting the fenugreek, the galactomannan has better solubility and higher viscosity, and part of the galactomannan is decomposed into mannan-oligosaccharide by adopting the micro-fermentation of mannase and galactosidase, so that the prepared galactomannan is easier to be absorbed and utilized by human bodies.

Description

一种从葫芦巴中制备半乳甘露聚糖的方法A method for preparing galactomannan from fenugreek

技术领域technical field

本发明属于天然食品添加剂技术领域,具体涉及一种从葫芦巴中制备半乳甘露聚糖的方法。The invention belongs to the technical field of natural food additives, in particular to a method for preparing galactomannan from fenugreek.

背景技术Background technique

半乳甘露聚糖是一种包含甘露糖骨干与半乳糖旁基的多糖,它以直线状(1-4)-连结的β-D型甘露糖骨干于它们的6-连接点连接到α-D型半乳糖的多糖,即1-6-连结的α-D型吡喃半乳糖。半乳甘露聚糖来源于胡芦巴胶,瓜尔豆胶,长角豆胶和他拉胶,不同植物来源的半乳甘露聚糖具有不同支化度。Galactomannan is a polysaccharide consisting of a mannose backbone and galactose side groups, which are linked to α- A polysaccharide of D-galactose, that is, 1-6-linked α-D-galactopyranose. Galactomannan is derived from fenugreek gum, guar gum, carob gum and tara gum, and galactomannan from different plant sources has different degrees of branching.

葫芦巴(拉丁学名:Trigonella foenum-graecum L.),是豆科胡卢巴属植物胡卢巴的习称。一年生草本植物,高30-80厘米,根系发达,茎直立,羽状三出复叶,叶柄平展,花期4-7月,果期7-9月。葫芦巴可以作为半乳甘露聚糖制备的原料,专利02138257.3公开了快速分散及速溶半乳甘露聚糖胶的生产方法。它是以优质工业级半乳甘露聚糖胶片(葫芦巴胶片)为原料,经水合、烘干、制粉、分级、食用酒精浸渍处理、离心脱溶、真空干燥制成。制成的半乳甘露聚糖胶全部溶解时间为25min,1%胶液粘度达到350mPa.s(170s-1),虽然溶解性能较其他植物种类来源的半乳甘露聚糖胶的溶解性能有所提高,但仍然不能满足人们对于快速溶解和提高粘度的要求。Fenugreek (Latin scientific name: Trigonella foenum-graecum L.) is the common name of fenugreek, a plant of the genus Fenugreek in the family Fabaceae. Annual herbaceous plant, 30-80 cm high, with well-developed root system, erect stem, pinnate three compound leaves, flat petiole, flowering period from April to July, and fruiting period from July to September. Fenugreek can be used as a raw material for the preparation of galactomannan, and patent 02138257.3 discloses a production method for rapid dispersion and instant galactomannan gum. It is made from high-quality industrial-grade galactomannan film (fenugreek film) through hydration, drying, milling, grading, soaking in edible alcohol, centrifugal precipitation, and vacuum drying. The total dissolution time of the prepared galactomannan gum is 25min, and the viscosity of 1% glue reaches 350mPa.s (170s -1 ), although the solubility is somewhat higher than that of galactomannan gum derived from other plant species. Improve, but still can not meet people's requirements for fast dissolution and increased viscosity.

发明内容Contents of the invention

本发明的目的在于提供一种从葫芦巴中制备半乳甘露聚糖的方法。The object of the present invention is to provide a method for preparing galactomannan from fenugreek.

一种从葫芦巴中制备半乳甘露聚糖的方法,按照如下步骤进行:A method for preparing galactomannan from fenugreek, carried out according to the following steps:

(1)将葫芦巴和胡里豆进行脱皮,然后加2-4%的水进行调质6-12min;(1) Peel the fenugreek and gourd beans, then add 2-4% water for conditioning for 6-12 minutes;

(2)将脱皮调质后的葫芦巴和胡里豆混合、破碎,过20-30目筛;然后进入砂磨机进行砂磨,过50-80目筛;(2) Mix and crush the fenugreek after peeling and conditioning, and pass through a 20-30 mesh sieve; then enter a sand mill for sand milling, and pass through a 50-80 mesh sieve;

(3)加入步骤(2)物料质量3-10倍的水,混合均匀,制成水溶液,加入甘露聚糖酶和半乳糖苷酶,水解,制成酶解液;(3) adding water 3-10 times the mass of the material in step (2), mixing evenly to make an aqueous solution, adding mannanase and galactosidase, hydrolyzing to make an enzymatic solution;

(4)沸水浴将步骤(3)制备的酶解液灭活后冷却至室温,过滤、脱色、浓缩得到糖浆;(4) Inactivate the enzymolysis solution prepared in step (3) in a boiling water bath and cool to room temperature, filter, decolorize, and concentrate to obtain syrup;

(5)将步骤(4)制备的糖浆经真空干燥即得半乳甘露聚糖。(5) Vacuum drying the syrup prepared in step (4) to obtain galactomannan.

所述葫芦巴和胡里豆的用量质量比为(2-5):1。The dosage-mass ratio of the fenugreek and the gourd beans is (2-5):1.

所述甘露聚糖酶的加入量为每克步骤(2)的混合物料100-200U。The added amount of the mannanase is 100-200U per gram of the mixed material in step (2).

所述半乳糖苷酶的加入量为每克步骤(2)的混合物料50-100U。The added amount of the galactosidase is 50-100 U per gram of the mixed material in step (2).

步骤(3)所述水解的温度为30-50℃,水解时间为1-5h。The hydrolysis temperature in step (3) is 30-50°C, and the hydrolysis time is 1-5h.

所述脱色采用活性炭脱色。The decolorization adopts active carbon decolorization.

所述真空干燥的温度为55-75℃,真空度为0.05-0.1MPa。The vacuum drying temperature is 55-75° C., and the vacuum degree is 0.05-0.1 MPa.

本发明的有益效果:本发明采用葫芦巴和胡里豆共同作为提取原料制备半乳甘露聚糖,相比单独采用葫芦巴得到的半乳甘露聚糖溶解性更好,粘度更高,采用甘露聚糖酶和半乳糖苷酶微发酵,部分半乳甘露聚糖分解为甘露寡糖,使得制备的半乳甘露聚糖更容易被人体吸收利用。Beneficial effects of the present invention: the present invention adopts fenugreek and gourd bean as extraction raw materials to prepare galactomannan, which has better solubility and higher viscosity than galactomannan obtained by using fenugreek alone. Enzyme and galactosidase micro-fermentation, part of the galactomannan decomposed into mannan oligosaccharides, making the prepared galactomannan easier to be absorbed and utilized by the human body.

附图说明Description of drawings

图1为葫芦巴与其他植物种子共提取后样品在水中溶解达到最大粘度的时间。Figure 1 shows the time for the sample to dissolve in water to reach the maximum viscosity after co-extraction of fenugreek and other plant seeds.

图2为葫芦巴与其他植物种子共提取后样品的粘度。Figure 2 shows the viscosity of samples after co-extraction of fenugreek and other plant seeds.

图3为葫芦巴与胡里豆不同质量比共提取后样品在水中溶解达到最大粘度的时间。Figure 3 shows the time for the samples to dissolve in water and reach the maximum viscosity after co-extraction of different mass ratios of fenugreek and gourd beans.

图4为葫芦巴与胡里豆不同质量比共提取后样品的粘度。Figure 4 shows the viscosity of samples after co-extraction of fenugreek and gourd beans in different mass ratios.

具体实施方式Detailed ways

为了便于理解本发明,下面将对本发明进行更全面的描述。但是,本发明可以以许多不同的形式来实现,并不限于本文所描述的实施例。相反地,提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。In order to facilitate the understanding of the present invention, the following will describe the present invention more fully. However, the present invention can be embodied in many different forms and is not limited to the embodiments described herein. On the contrary, these embodiments are provided to make the understanding of the disclosure of the present invention more thorough and comprehensive.

实施例1Example 1

一种从葫芦巴中制备半乳甘露聚糖的方法,按照如下步骤进行:A method for preparing galactomannan from fenugreek, carried out according to the following steps:

(1)将葫芦巴进行脱皮,然后加3%的水进行调质10min;(1) Peel the fenugreek, then add 3% water for conditioning for 10 minutes;

(2)将脱皮调质后的葫芦巴破碎,过25目筛;然后进入砂磨机进行砂磨,过60目筛;(2) Broken fenugreek after peeling and tempering, and crossed a 25-mesh sieve; then entered a sand mill for sand milling, and crossed a 60-mesh sieve;

(3)加入步骤(2)物料质量5倍的水,混合均匀,制成水溶液,加入甘露聚糖酶和半乳糖苷酶,水解,制成酶解液;所述甘露聚糖酶的加入量为每克步骤(2)的混合物料150U;所述半乳糖苷酶的加入量为每克步骤(2)的混合物料80U;所述水解的温度为45℃,水解时间为3h;(3) Add water with 5 times the mass of the material in step (2), mix uniformly to make an aqueous solution, add mannanase and galactosidase, and hydrolyze to make an enzymatic solution; the amount of mannanase added It is 150U of the mixed material per gram of step (2); the addition of the galactosidase is 80U of the mixed material of per gram of step (2); the temperature of the hydrolysis is 45°C, and the hydrolysis time is 3h;

(4)沸水浴将步骤(3)制备的酶解液灭活后冷却至室温,过滤、活性炭脱色、浓缩得到糖浆;(4) After inactivating the enzymolysis solution prepared in step (3) in a boiling water bath, cool to room temperature, filter, decolorize with activated carbon, and concentrate to obtain syrup;

(5)将步骤(4)制备的糖浆经真空干燥即得半乳甘露聚糖;所述真空干燥的温度为60℃,真空度为0.08MPa。(5) Vacuum drying the syrup prepared in step (4) to obtain galactomannan; the vacuum drying temperature is 60° C., and the vacuum degree is 0.08 MPa.

配置1%浓度的样品溶液;测定样品在水中溶解达到最大粘度的时间,达到最大粘度的标准为视觉看溶液为均一溶液,无气泡和结团,玻璃棒搅拌有阻力感,挑起后粘附5s内不掉落;测定溶解达到最大粘度的时间为38min;采用毛细管粘度计测定其粘度为352mPa.s(170s-1)。Configure a sample solution with a concentration of 1%; measure the time for the sample to dissolve in water to reach the maximum viscosity. The standard for reaching the maximum viscosity is that the solution is a uniform solution visually, without bubbles and agglomerates. The glass rod has a sense of resistance when stirred, and it adheres after stirring. It does not fall within 5s; the time to dissolve and reach the maximum viscosity is measured to be 38min; the viscosity is measured to be 352mPa.s (170s -1 ) by a capillary viscometer.

实施例2Example 2

为了提高半乳甘露聚糖的粘度,同时降低在水中溶解达到最大粘度的时间,发明人尝试采用其他含有半乳甘露聚糖的植物种子与葫芦巴共同提取,质量比为1:1,实验方法与实施例1相同,选用的植物包括海红豆、决明子、格木、胡里豆、椒麻、猪屎豆、翅荚木、田菁;配置1%浓度的样品溶液,测定样品在水中溶解达到最大粘度的时间及粘度,测定结果见图1和图2。In order to improve the viscosity of galactomannan and reduce the time to dissolve in water to reach the maximum viscosity, the inventor tried to use other plant seeds containing galactomannan and fenugreek to extract together, the mass ratio was 1:1, the experimental method Same as Example 1, the selected plants include sea red bean, cassia seed, gemu, gourd bean, pepper hemp, pig's dung bean, winged viburnum, and tianjing; a sample solution with a concentration of 1% is prepared, and the sample is dissolved in water to reach the maximum viscosity. The time and viscosity, measurement results are shown in Fig. 1 and Fig. 2.

由图1和图2可见,葫芦巴与胡里豆共同提取后的样品在水中溶解达到最大粘度的时间最短,粘度最大。It can be seen from Fig. 1 and Fig. 2 that the sample after co-extraction of fenugreek and gourd bean dissolves in water and reaches the maximum viscosity in the shortest time, and the viscosity is the largest.

实施例3提取配比优化Example 3 Extraction Proportion Optimization

选用葫芦巴与胡里豆作为共提取的原料,探索葫芦巴与胡里豆最佳用量比,设定葫芦巴与胡里豆的用量质量比为1:3、1:2、1:1、2:1、3:1、4:1、5:1、6:1,实验方法与实施例1相同;提取操作完成后,配置1%浓度的样品溶液,测定样品在水中溶解达到最大粘度的时间及粘度,结果见图3和图4。Fenugreek and gourd bean were selected as raw materials for co-extraction, the optimal dosage ratio of fenugreek and gourd bean was explored, and the dosage-mass ratio of fenugreek and gourd bean was set as 1:3, 1:2, 1:1, 2:1, 3: 1, 4:1, 5:1, 6:1, the experimental method is the same as in Example 1; after the extraction operation is completed, a sample solution with a concentration of 1% is prepared, and the time and viscosity of the sample dissolved in water to reach the maximum viscosity are measured, and the results are shown in Figures 3 and 4.

由图3和图4可见,葫芦巴与胡里豆的质量比为3:1时,样品在水中溶解达到最大粘度的时间最短,粘度最大。It can be seen from Figure 3 and Figure 4 that when the mass ratio of fenugreek to gourd bean is 3:1, the time for the sample to dissolve in water to reach the maximum viscosity is the shortest, and the viscosity is the largest.

实施例4Example 4

一种从葫芦巴中制备半乳甘露聚糖的方法,按照如下步骤进行:A method for preparing galactomannan from fenugreek, carried out according to the following steps:

(1)将葫芦巴和胡里豆进行脱皮,然后加3%的水进行调质10min;(1) Peel the fenugreek and gourd beans, then add 3% water for conditioning for 10 minutes;

(2)分别将脱皮调质后的葫芦巴和胡里豆破碎,按照质量比3:1混匀,过25目筛;然后进入砂磨机进行砂磨,过60目筛;(2) Break the peeled and tempered fenugreek and gourd beans respectively, mix according to the mass ratio of 3:1, and pass through a 25-mesh sieve; then enter the sand mill for sand grinding, and pass through a 60-mesh sieve;

(3)加入步骤(2)物料质量5倍的水,混合均匀,制成水溶液,加入甘露聚糖酶和半乳糖苷酶,水解,制成酶解液;所述甘露聚糖酶的加入量为每克步骤(2)的混合物料150U;所述半乳糖苷酶的加入量为每克步骤(2)的混合物料80U;所述水解的温度为45℃,水解时间为3h;(3) Add water with 5 times the mass of the material in step (2), mix uniformly to make an aqueous solution, add mannanase and galactosidase, and hydrolyze to make an enzymatic solution; the amount of mannanase added It is 150U of the mixed material per gram of step (2); the addition of the galactosidase is 80U of the mixed material of per gram of step (2); the temperature of the hydrolysis is 45°C, and the hydrolysis time is 3h;

(4)沸水浴将步骤(3)制备的酶解液灭活后冷却至室温,过滤、活性炭脱色、浓缩得到糖浆;(4) After inactivating the enzymolysis solution prepared in step (3) in a boiling water bath, cool to room temperature, filter, decolorize with activated carbon, and concentrate to obtain syrup;

(5)将步骤(4)制备的糖浆经真空干燥即得半乳甘露聚糖;所述真空干燥的温度为60℃,真空度为0.08MPa。(5) Vacuum drying the syrup prepared in step (4) to obtain galactomannan; the vacuum drying temperature is 60° C., and the vacuum degree is 0.08 MPa.

实施例5Example 5

一种从葫芦巴中制备半乳甘露聚糖的方法,按照如下步骤进行:A method for preparing galactomannan from fenugreek, carried out according to the following steps:

(1)将葫芦巴和胡里豆进行脱皮,然后加3%的水进行调质10min;(1) Peel the fenugreek and gourd beans, then add 3% water for conditioning for 10 minutes;

(2)分别将脱皮调质后的葫芦巴和胡里豆破碎,按照质量比4:1混匀,过25目筛;然后进入砂磨机进行砂磨,过60目筛;(2) Break the peeled and tempered fenugreek and gourd beans respectively, mix them evenly according to the mass ratio of 4:1, and pass through a 25-mesh sieve; then enter the sand mill for sand grinding, and pass through a 60-mesh sieve;

(3)加入步骤(2)物料质量6倍的水,混合均匀,制成水溶液,加入甘露聚糖酶和半乳糖苷酶,水解,制成酶解液;所述甘露聚糖酶的加入量为每克步骤(2)的混合物料200U;所述半乳糖苷酶的加入量为每克步骤(2)的混合物料100U;所述水解的温度为40℃,水解时间为3h;(3) Add water with 6 times the mass of the material in step (2), mix uniformly to make an aqueous solution, add mannanase and galactosidase, and hydrolyze to make an enzymatic solution; the amount of mannanase added It is 200U of the mixed material per gram of step (2); the addition of the galactosidase is 100U of the mixed material of per gram of step (2); the temperature of the hydrolysis is 40°C, and the hydrolysis time is 3h;

(4)沸水浴将步骤(3)制备的酶解液灭活后冷却至室温,过滤、活性炭脱色、浓缩得到糖浆;(4) After inactivating the enzymolysis solution prepared in step (3) in a boiling water bath, cool to room temperature, filter, decolorize with activated carbon, and concentrate to obtain syrup;

(5)将步骤(4)制备的糖浆经真空干燥即得半乳甘露聚糖;所述真空干燥的温度为60℃,真空度为0.06MPa。(5) Vacuum drying the syrup prepared in step (4) to obtain galactomannan; the vacuum drying temperature is 60° C., and the vacuum degree is 0.06 MPa.

实施例6Example 6

一种从葫芦巴中制备半乳甘露聚糖的方法,按照如下步骤进行:A method for preparing galactomannan from fenugreek, carried out according to the following steps:

(1)将葫芦巴和胡里豆进行脱皮,然后加3%的水进行调质10min;(1) Peel the fenugreek and gourd beans, then add 3% water for conditioning for 10 minutes;

(2)分别将脱皮调质后的葫芦巴和胡里豆破碎,按照质量比2:1混匀,过25目筛;然后进入砂磨机进行砂磨,过60目筛;(2) Break the peeled and tempered fenugreek and gourd beans respectively, mix them evenly according to the mass ratio of 2:1, and pass through a 25-mesh sieve; then enter the sand mill for sand grinding, and pass through a 60-mesh sieve;

(3)加入步骤(2)物料质量4倍的水,混合均匀,制成水溶液,加入甘露聚糖酶和半乳糖苷酶,水解,制成酶解液;所述甘露聚糖酶的加入量为每克步骤(2)的混合物料100U;所述半乳糖苷酶的加入量为每克步骤(2)的混合物料60U;所述水解的温度为50℃,水解时间为2h;(3) Add water with 4 times the mass of the material in step (2), mix uniformly to make an aqueous solution, add mannanase and galactosidase, and hydrolyze to make an enzymatic solution; the amount of mannanase added It is 100 U of the mixed material per gram of step (2); the addition amount of the galactosidase is 60 U of the mixed material of per gram of step (2); the temperature of the hydrolysis is 50°C, and the hydrolysis time is 2h;

(4)沸水浴将步骤(3)制备的酶解液灭活后冷却至室温,过滤、活性炭脱色、浓缩得到糖浆;(4) After inactivating the enzymolysis solution prepared in step (3) in a boiling water bath, cool to room temperature, filter, decolorize with activated carbon, and concentrate to obtain syrup;

(5)将步骤(4)制备的糖浆经真空干燥即得半乳甘露聚糖;所述真空干燥的温度为60℃,真空度为0.05MPa。(5) Vacuum drying the syrup prepared in step (4) to obtain galactomannan; the vacuum drying temperature is 60° C., and the vacuum degree is 0.05 MPa.

以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。The above-mentioned embodiments only express several implementation modes of the present invention, and the descriptions thereof are relatively specific and detailed, but should not be construed as limiting the patent scope of the invention. It should be pointed out that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent for the present invention should be based on the appended claims.

Claims (6)

1.一种从葫芦巴中制备半乳甘露聚糖的方法,其特征在于,按照如下步骤进行:1. a method for preparing galactomannan from Fenugreek, characterized in that, proceed according to the following steps: (1)将葫芦巴和胡里豆进行脱皮,然后加2-4%的水进行调质6-12min;(1) Peel the fenugreek and gourd beans, then add 2-4% water for conditioning for 6-12 minutes; (2)将脱皮调质后的葫芦巴和胡里豆混合、破碎,过20-30目筛;然后进入砂磨机进行砂磨,过50-80目筛;(2) Mix and crush the fenugreek after peeling and conditioning, and pass through a 20-30 mesh sieve; then enter a sand mill for sand milling, and pass through a 50-80 mesh sieve; (3)加入步骤(2)物料质量3-10倍的水,混合均匀,制成水溶液,加入甘露聚糖酶和半乳糖苷酶,水解,制成酶解液;(3) adding water 3-10 times the mass of the material in step (2), mixing evenly to make an aqueous solution, adding mannanase and galactosidase, hydrolyzing to make an enzymatic solution; (4)沸水浴将步骤(3)制备的酶解液灭活后冷却至室温,过滤、脱色、浓缩得到糖浆;(4) Inactivate the enzymolysis solution prepared in step (3) in a boiling water bath and cool to room temperature, filter, decolorize, and concentrate to obtain syrup; (5)将步骤(4)制备的糖浆经真空干燥即得半乳甘露聚糖;(5) Vacuum drying the syrup prepared in step (4) to obtain galactomannan; 所述葫芦巴和胡里豆的用量质量比为(2-5):1。The dosage-mass ratio of the fenugreek and the gourd beans is (2-5):1. 2.根据权利要求1所述从葫芦巴中制备半乳甘露聚糖的方法,其特征在于,所述甘露聚糖酶的加入量为每克步骤(2)的混合物料100-200U。2. The method for preparing galactomannan from Fenugreek according to claim 1, characterized in that the amount of mannanase added is 100-200 U per gram of the mixed material in step (2). 3.根据权利要求1所述从葫芦巴中制备半乳甘露聚糖的方法,其特征在于,所述半乳糖苷酶的加入量为每克步骤(2)的混合物料50-100U。3. The method for preparing galactomannan from Fenugreek according to claim 1, characterized in that the amount of galactosidase added is 50-100 U per gram of the mixed material in step (2). 4.根据权利要求1所述从葫芦巴中制备半乳甘露聚糖的方法,其特征在于,步骤(3)所述水解的温度为30-50℃,水解时间为1-5h。4 . The method for preparing galactomannan from Fenugreek according to claim 1 , wherein the hydrolysis temperature in step (3) is 30-50° C., and the hydrolysis time is 1-5 h. 5.根据权利要求1所述从葫芦巴中制备半乳甘露聚糖的方法,其特征在于,所述脱色采用活性炭脱色。5. The method for preparing galactomannan from Fenugreek according to claim 1, wherein said decolorization adopts active carbon decolorization. 6.根据权利要求1所述从葫芦巴中制备半乳甘露聚糖的方法,其特征在于,所述真空干燥的温度为55-75℃,真空度为0.05-0.1MPa。6 . The method for preparing galactomannan from Fenugreek according to claim 1 , wherein the vacuum drying temperature is 55-75° C., and the vacuum degree is 0.05-0.1 MPa.
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