JP4560635B2 - Sericin separation and recovery equipment - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an apparatus for obtaining high-molecular-weight sericin from silk fibers with high yield.
[0002]
[Prior art]
Various attempts have been made to effectively use silk sericin. In particular, as disclosed in JP-A-11-131318, a scouring solution obtained by high-temperature and high-pressure treatment of silk fibers with high-temperature water is frozen and thawed. Thus, it is also known that high molecular weight sericin can be separated and recovered. However, in order to carry out this method efficiently, it is necessary to carefully control the freezing and thawing process, and it has not been possible to carry out industrially with a conventional freezing apparatus or the like.
[0003]
[Problems to be solved by the invention]
A high-molecular-weight sericin having a molecular weight of 100,000 or more is stabilized by freezing and thawing a scouring solution obtained by treating silk fiber with high-temperature and high-pressure water at high temperature and pressure, that is, a sericin aqueous solution. It has been found that the sericin aqueous solution should be slowly frozen for about 8 hours or longer, and then cooled to -10 ° C. or lower to complete the freezing. Therefore, the present invention provides an apparatus that can freeze a sericin aqueous solution uniformly and gently over 8 hours at around 0 ° C., and that can perform processes before and after freezing with very good workability and without waste. The task is to do.
[0004]
[Means for Solving the Problems]
In the present invention, a jacket having a silk fiber scouring liquid inlet at the lower end and a manifold having a large number of vertical pipes on the upper surface are installed in the jacket having heat insulation and heat insulation properties, and the manifold is introduced and stored in this vertical pipe. The above problem was solved by freezing and thawing the scouring liquid in the jacket. The freezing temperature of the scouring solution can be controlled by air cooling.
[0005]
That is, in the present invention, for example, a scouring solution containing about 0.2 to 2.5% of sericin can be stored in divided tubes in the vertical pipe and frozen by air cooling using a refrigeration condenser or the like. The method of gradually freezing at a liquid temperature of about 0 ° C. over 8 hours and then cooling the liquid temperature to about −10 ° C. or lower to complete the freezing can be carried out very efficiently and uniformly. In addition, the frozen scouring solution can be efficiently thawed as it is in the jacket.
[0006]
The vertical tube is preferably set to have a diameter of 500 mm or less for the purpose of uniformly and gradually freezing the scouring solution, but preferably has a diameter of 50 to 300 mm, particularly about 70 to 200 mm.
[0007]
The standing tube group for storing, freezing and thawing the scouring liquid in the jacket is preferably present in a state surrounded by the partition plate, and the lower end of the partition plate is spaced apart from the upper surface of the manifold by a certain distance. It should be positioned in an open state. In this case, the cold air sent by the refrigeration condenser or the like flows in the inside of the jacket through a flow path that flows from the upper side to the lower side of the vertical pipe inside the partition plate and exits between the lower end of the partition plate and the inner wall of the jacket. It comes to circulate.
[0008]
Note that the temperature of the cool air in the jacket needs to be stably controlled at about 0 ° C. to −6 ° C. so that the scouring liquid in the vertical tube is frozen at around 0 ° C. for a long time. In general, a refrigeration condenser is preferably used, and a refrigeration condenser and a heating condenser may be used in combination.
[0009]
The scouring solution frozen in the vertical pipe is thawed as it is, and this thawing may be carried out with warm air using a heating condenser, but is preferably carried out using hot water. Therefore, it is recommended to provide a hot water inlet at the bottom of the jacket, and the hot water introduced into the jacket is controlled by a liquid level sensor so that the water level is automatically adjusted at a certain height not exceeding the vertical pipe. It is better.
[0010]
DETAILED DESCRIPTION OF THE INVENTION
Next, the present invention will be described in more detail with reference to an example shown in the drawings.
The apparatus shown in FIG. 1 has a jacket 1 having heat insulation and heat insulation, and a manifold 4 having a silk fiber scouring fluid inlet 2 at its lower end and a plurality of vertical tubes 3 on its upper surface. The refrigeration condenser 5 is installed above the vertical pipe 3, and the cool air from the refrigeration condenser 5 is sent downward by the fan 7, and the scouring liquid introduced and stored in the vertical pipe 3 is supplied with this cold air. To freeze.
[0011]
In this example, the diameter of the vertical pipe 3 in the jacket is 80 mm, the vertical pipe 3 is surrounded by the partition plate 8 and exists in the jacket, and the lower end of the partition plate 8 is the bottom of the manifold 4. It is located in a state where it is spaced apart from the upper surface, and the cold air from the refrigeration condenser 5 descends while uniformly cooling the inside of the partition plate 8 and the periphery of the vertical pipe 3, and the lower end of the partition plate 8 and the manifold From between the upper surface of 4, it comes out between the jacket 1 and the partition plate 8, rises there, and circulates in the jacket 1.
[0012]
The refrigeration condenser 5 is controlled so that the cold air is kept at about 0 to -6 ° C. and the scouring liquid in the vertical tube 3 is frozen at a temperature around 0 ° C. over a long period of time. This temperature control can be carried out by using together with a heating condenser 6 provided above 5.
[0013]
The scouring liquid in the vertical pipe 3 is frozen at around 0 ° C. for a long time, and then cooled to −10 ° C. or lower to complete the freezing. As a result, high molecular weight sericin having a molecular weight of 100,000 or higher can be precipitated. And This sericin thaws the scouring solution in the vertical tube 3, removes the thawing solution, and separates it with a centrifuge, and the thawing solution is taken out through the scouring fluid inlet 2 of the manifold 4. ing.
[0014]
In this apparatus, hot water at around 50 ° C. is used to efficiently thaw the frozen scouring liquid, and a hot water inlet 9 is provided on the bottom surface of the jacket 1. The height of the introduced hot water is controlled by the liquid level sensor 10a so as to be maintained near the mouth of the vertical pipe 3 in the jacket 1. Usually, hot water at around 50 ° C. is exchanged about 3 times in the jacket, the frozen scouring liquid is made fluid, and it is taken out from the scouring liquid inlet 2 to the centrifuge as a thawing liquid. ing.
[0015]
Furthermore, this apparatus is provided with a liquid level sensor 10b for controlling the amount of scouring liquid introduced (controlling the liquid level near the mouth of the vertical pipe 3). It is preferable to prepare an amount of scouring liquid suitable for the volume, and to introduce it every time. This is because freezing and thawing are performed in a completely shielded state in the vertical pipe 3.
[0016]
Since the high molecular weight sericin contained in the thawing solution adheres to the wall surfaces of the vertical pipe 3 and the manifold 4 and hardly flows out completely, in this apparatus, the upper part of the vertical pipe 3 and / or the side surface of the manifold 4 is washed. A nozzle 11 for water is attached, and high pressure water is sprayed to recover the remaining sericin.
[0017]
Next, the usage example of this apparatus is shown.
The silk fabric 3 was scoured at 60 ° C. for 30 minutes and then scoured at 120 ° C. for 30 minutes without chemicals to obtain 150 liters of a scouring solution having a sericin content of 0.3%.
The apparatus shown in FIG. 1 was refrigerated in advance, the temperature in the jacket was lowered to about 0 to 5 ° C., and 150 liters of the scouring liquid was introduced into the vertical pipe 3 from the scouring liquid inlet 2. Thereafter, the operation and stop of the refrigeration compressor are time-controlled, and the liquid temperature in the vertical pipe 3 is gradually frozen from + 5 ° C. to −2 ° C. over about 10 hours as shown in FIG. Frozen below 10 ° C. The temperature around the vertical pipe 3 is controlled to be maintained at about -5 ° C to -7 ° C for the first 8 hours and then cooled to -15 ° C.
[0018]
When freezing is completed, hot water at 50 ° C. is introduced from the hot water inlet 9 of the jacket 1, and the frozen scouring liquid in the vertical tube 3 is thawed. The hot water is controlled by the liquid level sensor 10a, introduced to the vicinity of the mouth of the vertical pipe 3, held for a certain period of time, and discharged three times to thaw the scouring liquid in the vertical pipe 3 and introduce the scouring liquid. After pumping from the port 2 to the centrifuge, high pressure water was sprayed through the nozzle 11 in the vertical pipe and the manifold, and the remaining sericin was recovered.
[0019]
The thawed solution thus obtained was dehydrated with a centrifuge and dried. As a result, 282 g of sericin having a molecular weight of 129,000 (recovery rate: 63.5%) could be obtained.
[0020]
【The invention's effect】
In the apparatus of the present invention, high molecular weight sericin can be produced from silk fibers (raw silk, etc.) with good operability. Since the freezing temperature of the scouring solution can be controlled by air cooling, the freezing time can be easily maintained constant, and high-molecular weight sericin can be recovered stably and with good reproducibility. In addition, there is an effect that the scouring solution can be efficiently frozen and thawed in the same apparatus.
[Brief description of the drawings]
FIG. 1 is an explanatory diagram showing an example of an apparatus according to the present invention.
FIG. 2 is a graph showing temperature changes in an example of use of the apparatus of the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Jacket 2 Scouring liquid inlet 3 Stand pipe 4 Manifold 5 Refrigeration condenser 6 Heating condenser 7 Fan 8 Partition plate 9 Hot water inlet 10a, 10b Liquid level sensor 11 Nozzle

Claims (4)

A jacket with a silk fiber scouring fluid inlet at the lower end and a large number of vertical pipes on the upper surface is installed in a jacket having heat insulation and heat insulation properties. For freezing and thawing the sericin in the jacket, wherein the freezing temperature of the scouring solution is controlled by air cooling. The standing pipe group is present in the jacket in a state surrounded by a partition plate, and the lower end of the partition plate is positioned in a state of being spaced apart from the upper surface of the manifold. The apparatus of claim 1. The apparatus according to claim 1 or 2, wherein the freezing temperature is temperature-controlled by a refrigeration condenser or a combination of a refrigeration condenser and a heating condenser. The apparatus according to any one of claims 1 to 3, wherein a hot water inlet for introducing hot water for thawing the sericin aqueous solution frozen in the vertical pipe is provided below the jacket.

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