WO2005123813A1

WO2005123813A1 - Powdery vinyl pyrrolidone polymer

Info

Publication number: WO2005123813A1
Application number: PCT/JP2005/010803
Authority: WO
Inventors: Keiichi Fujise; Tomiyasu Ueta
Original assignee: Dai-Ichi Kogyo Seiyaku Co., Ltd.; Nippon Shokubai Co., Ltd.
Priority date: 2004-06-17
Filing date: 2005-06-13
Publication date: 2005-12-29
Also published as: JP2006002047A

Abstract

A vinyl pyrrolidone polymer which, even when used as a binder in a reduced amount in tablet production, does not necessitate any additional complicated step and has no fear of resulting in a reduced tableting yield. The polymer is a powdery vinyl pyrrolidone polymer at least 90 wt.% of which is accounted for by particles having a particle diameter of 35 μm or smaller. The average particle diameter of the polymer preferably is 20 μm or smaller. This powdery vinyl pyrrolidone polymer is obtained by drying an aqueous vinyl pyrrolidone polymer solution having a concentration of 5-40 wt.% with a two-fluid-nozzle type spray drier.

Description

Specification

Powdered pyrpyrrolidone polymer

Technical field

[0001] The present invention relates to a powdery vinylpyrrolidone polymer, and in particular, to the field of cosmetics such as pharmaceutical auxiliaries (such as pharmaceuticals, health foods, quasi-drugs or additives in soft drinks), hair care products, and the like. Also, the present invention relates to a powdery bulpyrrolidone polymer suitably used in a wide range of fields such as various special industrial uses such as a dye auxiliary.

Background art

[0002] It is already known to use a vinylpyrrolidone polymer as a binder when producing a solid preparation such as a tablet (for example, Patent Documents 1 and 2).

Patent Document 1: JP-A-5-32554 (paragraphs [0012] to [0016])

Patent Document 2: Japanese Patent Application Laid-Open No. 2000-351732 (Claim 3)

Disclosure of the invention

Problems to be solved by the invention

[0003] Since this vinylpyrrolidone polymer is expensive, it is necessary to reduce the amount of use as much as possible. If the amount used (blended amount) is simply reduced, the problem that the tableting rate (the rate at which the tablet can be completely molded without chipping) is naturally reduced. To avoid this problem, various complicated steps were required. In other words, the smaller the amount of the vinylpyrrolidone polymer used, the more necessitating the spraying of water or an organic solvent at the time of mixing the powder, or forming the granules once and then compressing the tablets. The complicated process of performing the molding became necessary.

[0004] The present invention has been made in view of the above-mentioned circumstances, and its object is to provide a method for use in various fields, for example, when used as a binder in the production of solid preparations such as tablets. It is an object of the present invention to provide a vinylpyrrolidone polymer having a special action and effect such that even if the amount used is reduced, there is no need to perform other complicated steps and there is no concern that the tableting rate is reduced. .

Means for solving the problem [0005] The present inventor has limited the particle size of the bulpyrrolidone polymer used, so that even if a small amount of the compound is used, the tableting rate is not reduced, and if the tableting rate is not reduced, the strength is improved. The present inventors have found that the disintegration time of the preparation is prolonged, which led to the present invention.

That is, the powdery vinylpyrrolidone polymer of the present invention (hereinafter, also referred to as “powder polymer” or simply “polymer”) contains 70% by weight or more of particles having a particle diameter of 35 μm or less. Suppose.

[0007] The powdery polymer of the present invention more preferably contains 90% by weight or more of particles having a particle diameter of 35 µm or less!

[0008] The powdery polymer of the present invention preferably has an average particle size of 20 µm or less.

[0009] The powdery polymer of the present invention is a polymer as described above, and preferably has a K value of 40 or less.

[0010] The bulletpyrrolidone polymer used in the present invention is a homopolymer of N-bul-2-pyrrolidone.

The invention's effect

[0011] According to the powdery vinylpyrrolidone polymer of the present invention, pharmaceutical auxiliaries (such as additives in health foods, quasi-drugs or soft drinks, etc., in addition to pharmaceuticals), cosmetics fields such as hair care products, Also, it can be suitably used in a wide range of fields such as various special industrial uses such as dye auxiliaries. For example, when used as a binder in the manufacture of solid preparations such as tablets and granules, even if the amount used is reduced, there is no need for additional complicated steps and there is a concern that the tableting rate may be reduced. Therefore, even if the polymer is used in other fields, it is possible to reduce the amount of the powder of the polymer which is expensive, thereby enabling cost reduction.

BEST MODE FOR CARRYING OUT THE INVENTION

The powdery polymer of the present invention contains 70% by weight or more of particles having a particle diameter of 35 μm or less. If the amount is less than 70% by weight, the compounding amount cannot be reduced, for example, when this is used as a binder in the production of a solid preparation such as a tablet. That is, when it is less than 70% by weight, when used as a binder, the effective tableting rate is reduced. When 90% by weight or more of particles having a particle size of 35 m or less are contained, an extremely good tableting ratio is obtained, and the obtained tablets The disintegration time is also prolonged, and the amount of the powder of the polymer, which is expensive, can be reduced, and the cost can be reduced.

[0013] In addition to the above configuration, when the particles constituting the powder have an average particle size of 20 μm or less, the tableting rate can be more effectively improved, and the powder is expensive. The amount of powder used for coalescence can be further reduced, thereby further reducing costs.

In the present invention, by using a two-fluid nozzle (pressurized two-fluid nozzle) type spray dryer, 70% by weight or more of particles having a particle diameter of 35 μm or less and an average particle diameter of 20% or less are used. A powder polymer consisting of particles of not more than μm is obtained. The drying mechanism of the two-fluid nozzle spray dryer is described in detail, for example, in Japanese Patent No. 3034974 and Japanese Patent No. 3155028. Spray dryers include horizontal cocurrent type, vertical descent cocurrent type, vertical ascending countercurrent type, vertical descent mixing type, vertical ascent mixing type, etc. from the viewpoint of the flow direction of hot air spray droplets. However, any spray dryer may be used. Further, the two-fluid nozzle is a right-angle type in which a liquid flow and a gas flow collide with each other at right angles (perpendicular to each other) to form fine particles, and a parallel flow type (internal mixing type) in which a liquid flow and a gas flow are jetted in parallel. , External mixing type), but any type may be used.

[0015] The concentration of the aqueous polymer solution used when producing the powder polymer using the two-fluid nozzle spray dryer is not particularly limited, but is preferably 5 to 40% by weight. If the content is less than 5% by weight, the production cost becomes high and there is a possibility of causing economic disadvantage. On the other hand, if it exceeds 40% by weight, a problem arises in that a desired powdery vinylpyrrolidone polymer cannot be obtained. Incidentally, a more preferable range is 10 to 30% by weight.

Further, it is preferable that the K value of the aqueous solution is 40 or less. If the K value exceeds 0, a powdery polymer is not obtained. A more preferred K value is 35 or less, most preferably 30 or less.

[0017] The K value is a constant that indicates the degree of polymerization proposed by the German chemist H. Fikenture, and is established over a wide range in a polymer solution.

[0018] The K value of the bulpyrrolidone polymer solution can be determined by the following measurement method. That is, if the K value is less than 20, measure the viscosity of the 5% (g / 100 ml) solution, and if the K value is 20 or more, measure the viscosity of the l% (gZlOOml) solution. Sample concentration is dry Convert things. Therefore, if the K value is less than 20, sample 5.0 g.If the K value is 20 or more, accurately weigh Og, put it in a 100 ml volumetric flask, add distilled water at room temperature, and shake. While making complete dissolution, whisk distilled water to make exactly 100ml. After leaving this sample solution in a constant temperature bath (25 ± 0.2 ° C) for 30 minutes, measure the time for the solution to flow between the two marked lines using an Ubbelohde viscometer. The measurement is performed several times and the average value is taken. Measure the same for distilled water to determine the relative viscosity. The two flow times obtained are corrected based on the Hagen bach-Couette correction values.

[Number 1]

_ V "300C log Z + (C + 1 .5C lo9 Z) ² +1 .5 C logZ-C

0.15 C + 0.003C ²

In the above formula, Z represents the relative viscosity (η rel) of the solution having the concentration C, C represents the concentration (%: gZ100 ml), and the relative viscosity Z is obtained by the following formula;

Z (r? Rel) = (flow time of solution) ÷ (flow time of water)

[0020] By employing the powdered vinylpyrrolidone polymer of the present invention, the amount of powder used can be reduced, thereby enabling cost reduction in various fields. Specifically, when used as a binder in the manufacture of a solid preparation, for example, a tablet, the amount used can be reduced, and even if the amount is reduced, for example, the tableting rate does not decrease, and the tablet disintegrates. The time can be extended. In other words, conventionally, when a bulpyrrolidone polymer was used as a binder, 5 to 20% by weight was contained in the preparation, but by using the powdery polymer of the present invention, the content in the preparation was increased. it is possible to suppress the rate to 1 to 3 wt ^_0/0. Since it is an expensive bulpyrolidone polymer, it has economical benefits and also has the effect of extending the disintegration time as described above.

Example

Examples of the present invention will be described below, but the present invention is not limited thereto.

Example 1 (Production of Polymer [A])

Bullpyrrolidone polymer with a K value of 29.8 (N-Bull-2-pyrrolidone homopolymer) 2 The 0% by weight aqueous solution was dried with a two-fluid nozzle spray dryer (L-12 (*) type, manufactured by Okawara Kakoki Co., Ltd.) to obtain a powdery vinylpyrrolidone polymer [A].

[0023] Drying conditions were as follows: two-fluid nozzle liquid cap orifice: 3. Omm, air cap orifice: 1.5 mm, air pressure: 2. Okg / cm ² , heat input temperature: 170 ° C, exhaust temperature: 110 ° C, Throughput: 4 L / min and 7 pieces.

The powdery pyrpyrrolidone polymer [A] contained 76% by weight of particles having a particle size of 35 μm or less, and had an average particle size of 19.

Example 2 (Production of Polymer [B])

Bullpyrrolidone polymer with a K value of 17.5 (N-Bulle-2-pyrrolidone homopolymer) 3

The 5% by weight aqueous solution was dried with a two-fluid nozzle spray dryer (L-12 (*) type, manufactured by Okawara Kakoki Co., Ltd.) to obtain a powdery vinylpyrrolidone polymer [B].

[0026] Drying conditions were as follows: two-fluid nozzle liquid cap orifice: 3. Omm, air cap orifice:

1.5mm, air pressure: 2. Okg / cm ² , heat input temperature: 230 ° C, exhaust temperature: 110 ° C, throughput: 7

7 with L / min.

[0027] The obtained powdery pyrpyrrolidone polymer [B] contained 91% by weight of particles having a particle size of 35 µm or less, and had an average particle size of 18. O / zm.

[Comparative Example 1 (Production of polymer [a])]

Bullpyrrolidone polymer with a K value of 29.8 (N-Bulle-2-pyrrolidone homopolymer) 2

The 0% by weight aqueous solution was dried and powdered by a disk atomizer set spray dryer to obtain a powdery vinylpyrrolidone polymer [a].

[0029] Drying conditions were as follows: disk peripheral speed 85mZsec, processing speed: 280L / min, heat input temperature: 170 ° C

, Exhaust temperature: 110 ° C.

[0030] The obtained powdered pyrpyrrolidone polymer [a] contained 9% by weight of particles having a particle size of 75 µm or less, and had an average particle size of 159 µm.

[Evaluation Examples 1-2 and Comparative Evaluation Example 1]

A total of 300 g of the formulation shown in the following [Table 1] was put in a plastic bag and mixed for 30 seconds. After that, tableting was performed according to a conventional method. The tableting conditions are as follows.

[0032] (Tabletting conditions) Tablet weight: 3.5gZ tablet, tablet diameter: 8mm in diameter, tablet pressure: 500kg, tablet machine: rotary type tablet machine HT-9 (manufactured by Hata Iron Works)

[0033] [Table 1]

[0034] The tableting rate and disintegration time of the obtained tablet were evaluated as follows.

(Evaluation of tableting rate and disintegration time)

The (good) tableting rate at the time of producing the tablet and the disintegration time of the obtained tablet were evaluated. Good tableting rate (%): The rate of formation of tablets that could be perfectly molded was determined.

Disintegration time (seconds): Tested according to the 14th revision of the Japanese Pharmacopoeia, and the time required for the tablet to completely dissolve was measured.

The results are shown in [Table 2] below.

[Table 2] Example Example Comparative

1 2 1 Symbol of polymer used [A] [B] [a] Drying method Two-fluid Two-fluid disc

(Drying model) Nozzle Nozzle atomizer

75wm or less (weight%) Θ

35 or less (weight%) 76 9 1 Average particle size C // m) 1 9. 1 1 8. O 15 9 Good tableting ratio (%) 96 98 78 Collapse at break (sec) 253 2 66 1 78 Industrial Applicability

The powdery vinylpyrrolidone polymer of the present invention may be used as a pharmaceutical auxiliary (additives in health foods, quasi-drugs or soft drinks, etc. in addition to pharmaceuticals), in the cosmetics field such as hair care products, and as a dye auxiliary. Are used for various special industrial applications.

Claims

The scope of the claims

[1] A powdered vinylpyrrolidone polymer containing 70% by weight or more of particles having a particle size of 35 μm or less.

[2] A powdered vinylpyrrolidone polymer containing 90% by weight or more of particles having a particle size of 35 μm or less.

[3] The powdery pyrpyrrolidone polymer according to claim 1 or 2, wherein the average particle diameter is 20 µm or less.

[4] The powdery bulpyrrolidone polymer according to any one of claims 1 to 3, wherein the K value is 40 or less.