CN114456556B - Polyhydroxyalkanoate tablet and preparation method and application thereof - Google Patents
Polyhydroxyalkanoate tablet and preparation method and application thereof Download PDFInfo
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- CN114456556B CN114456556B CN202210036353.1A CN202210036353A CN114456556B CN 114456556 B CN114456556 B CN 114456556B CN 202210036353 A CN202210036353 A CN 202210036353A CN 114456556 B CN114456556 B CN 114456556B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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Abstract
The invention relates to the technical field of degradable material processing, and in particular discloses a polyhydroxyalkanoate tablet, a preparation method and application thereof, wherein the polyhydroxyalkanoate tablet comprises the following components: polyhydroxyalkanoates, maltodextrins, carboxymethyl starch, starch octenyl succinate, lubricants. The polyhydroxyalkanoate tablet prepared by the method has the advantages of high hardness, strength, low friability and smooth surface, the tablet shape is favorable for subsequent processing, use, storage and transportation, and the cold pressing technology is adopted in the preparation process, so that the performance of polyhydroxyalkanoate is not influenced.
Description
Technical Field
The invention belongs to the technical field of degradable material processing, and particularly relates to a polyhydroxyalkanoate tablet, a preparation method and application thereof.
Background
Polyhydroxyalkanoate is a natural high molecular biological material, is intracellular polyester synthesized by microorganisms, and can be fermented to produce polyhydroxyalkanoate materials with different structures and performances, such as poly-3-hydroxybutyrate (P-3 HB), poly-4-hydroxybutyrate (P-4 HB), poly-3-hydroxybutyrate valerate (PHBV), poly-3-hydroxybutyrate caproate (PHBH), poly-3-hydroxybutyrate-4-hydroxybutyrate P (3 HB-co-4 HB) and the like by changing strains, carbon source types and technological conditions in the culture process, so as to meet the requirements of different industries. The polyhydroxyalkanoate has good biocompatibility and biodegradability, so that the polyhydroxyalkanoate can be used for preparing biodegradable plastics.
The polyhydroxyalkanoate obtained by washing and drying the P-3HB extracted from the cell body is in the form of powder, and the powder raw material is unfavorable for the existing processing technique and storage, transportation and use, and has lower efficiency and utilization than the granular or flaky raw material. However, at present, the preparation process of the polyhydroxyalkanoate tablet mainly has the following problems: (1) A screw extruder or other heating machines are usually adopted to process the polyhydroxyalkanoate powder, but the processing window of the polyhydroxyalkanoate is sensitive and narrow, so that the high temperature can crack the long chain molecular chain of the polyhydroxyalkanoate, degrade and reduce the molecular weight, thereby influencing the material performance of the polyhydroxyalkanoate; (2) When the polyhydroxyalkanoate powder is used in a conventional tablet press machine (cold pressing process), the polyhydroxyalkanoate powder has extremely poor fluidity, so that the cold-pressed tablet is incomplete in shape and easy to disperse under stress, and the polyhydroxyalkanoate tablet can be dispersed into powder in the storage and transportation processes.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides a polyhydroxyalkanoate tablet, a preparation method and application thereof, wherein the polyhydroxyalkanoate tablet has high hardness, strength, low friability and smooth surface, the tablet shape is beneficial to subsequent processing, use, storage and transportation, and the cold pressing process is adopted in the preparation process, so that the performance of polyhydroxyalkanoate is not influenced.
In a first aspect of the invention, there is provided a polyhydroxyalkanoate tablet comprising the following components: polyhydroxyalkanoates, maltodextrins, carboxymethyl starch, starch octenyl succinate, lubricants.
In some embodiments of the invention, the polyhydroxyalkanoate comprises 60-80%, preferably 60-70% by weight of the polyhydroxyalkanoate tablet.
In some embodiments of the invention, the maltodextrin comprises 1-10%, preferably 5-10% by weight of the polyhydroxyalkanoate tablet.
Maltodextrin, which is a tablet adjuvant prepared by modifying starch, is also a biodegradable material and can be used as an excipient.
In some embodiments of the invention, the carboxymethyl starch comprises 1-10%, preferably 5-10% by weight of the polyhydroxyalkanoate tablet.
Carboxymethyl starch is a modified starch with anions, which can be better combined with polyhydroxyalkanoate due to the existence of negative charges.
In some embodiments of the invention, the starch octenyl succinate comprises 1-15%, preferably 10-15% by weight of the polyhydroxyalkanoate tablet.
The octenyl succinic acid starch ester is commonly called as a pure gum, is modified starch obtained by introducing hydrophilic and oleophylic amphoteric groups on a starch molecular chain, has stable property and biodegradability, and can be matched with polyhydroxyalkanoate. In addition, the octenyl succinic acid starch ester has good emulsification stability and thickening effect, can increase the whiteness and surface gloss of the product, and improves the fluidity of the product. Meanwhile, the tablet has good shaping and bonding effects, ensures the volume stability of the tablet, reduces the dosage deviation of the polyhydroxyalkanoate and improves the compression molding property of the polyhydroxyalkanoate.
In some embodiments of the invention, the lubricant comprises 1-15%, preferably 10-15% by weight of the polyhydroxyalkanoate tablet.
In some embodiments of the present invention, the lubricant comprises at least one of stearic acid, magnesium stearate, colloidal silica, talc, calcium carbonate, sodium bicarbonate, polyethylene glycols, magnesium lauryl sulfate; magnesium stearate and calcium carbonate are preferred.
In some embodiments of the invention, the polyhydroxyalkanoate tablet comprises the following components in parts by weight:
60-80 parts of polyhydroxyalkanoate;
1-10 parts of maltodextrin;
1-10 parts of carboxymethyl starch;
1-15 parts of octenyl succinic acid starch ester;
1-15 parts of lubricant.
In some preferred embodiments of the present invention, the polyhydroxyalkanoate tablet comprises the following components in parts by weight:
60-70 parts of polyhydroxyalkanoate;
5-10 parts of maltodextrin;
5-10 parts of carboxymethyl starch;
10-15 parts of octenyl succinic acid starch ester;
10-15 parts of lubricant.
In some preferred embodiments of the present invention, the polyhydroxyalkanoate tablet comprises the following components in parts by weight:
70 parts of polyhydroxyalkanoate;
5 parts of maltodextrin;
5 parts of carboxymethyl starch;
10 parts of octenyl succinic acid starch ester;
5 parts of magnesium stearate;
5 parts of calcium carbonate.
In a second aspect of the present invention, there is provided a method for producing the above polyhydroxyalkanoate tablet, comprising the steps of:
and (3) drying the polyhydroxyalkanoate, maltodextrin, carboxymethyl starch, starch octenyl succinate and lubricant, uniformly mixing according to a proportion, and stamping to prepare tablets.
In some embodiments of the invention, the number of presses is 3-6.
In some embodiments of the invention, the pressure used for the stamping is in the range of 40-60KN, e.g., 40-55KN, 40-50KN, 45-60KN, 45-55KN, 45-50KN, 50-60KN, 50-55KN.
In some embodiments of the invention, the tablet has a diameter in the range of 3-25mm, such as 3-20mm, 3-15mm, 3-10mm, 3-5mm; the thickness of the tablet ranges from 3 to 8mm, for example from 3 to 7mm, from 3 to 6mm, from 3 to 5mm.
In a third aspect, the present invention provides the use of the polyhydroxyalkanoate tablets described above in the fields of food packaging, cosmetic packaging and pharmaceutical packaging.
The polyhydroxyalkanoate tablet according to the embodiment of the invention has at least the following beneficial effects:
(1) The invention endows the polyhydroxyalkanoate tablet with high adhesive force, high forming degree, excellent hardness, strength and friability through the compounding of maltodextrin, carboxymethyl starch and octenyl succinic acid starch ester, is suitable for direct tabletting and other performances, and is beneficial to the application of subsequent processed products;
(2) The invention uses specific auxiliary materials, and after repeated stamping and auxiliary feeding, the fluidity and viscosity of the polyhydroxyalkanoate powder are increased, thus obviously improving the problem of difficult blanking;
(3) The invention adopts a cold pressing processing mode, and the polyhydroxyalkanoate powder is only externally applied with a certain pressure, so that the molecular chain structure is not damaged, the performance of the polyhydroxyalkanoate material is well reserved, and the subsequent processing is facilitated; in addition, the components used in the invention are all inorganic auxiliary agents or modified starch, and the degradation performance of polyhydroxyalkanoate is not affected;
(4) The invention has lower cost.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
Examples
The polyhydroxy fatty acid ester used in the invention is purchased from the company of Ma De Sheng technology Co., ltd., maltodextrin is purchased from Shandong's Methoxychemical Co., ltd., carboxymethyl starch is purchased from Guangdong Hongxin Biotechnology Co., ltd., and octenyl succinic acid starch ester is purchased from Kang Disi chemical industry.
The amounts of the components of examples 1 to 5 and comparative examples 1 to 4 in the present invention are shown in Table 1.
Table 1 (Unit: parts by weight)
The polyhydroxyalkanoate tablets of examples 1-5 and comparative examples 1-4 were prepared as follows:
firstly, all the components are pretreated and put into a vacuum microwave drying oven for drying, so that the moisture of the powder material is not more than 0.5%. And then the components are put into a three-dimensional mixer according to the proportion and are mixed uniformly. The evenly mixed powder is put into a feeding cylinder of a high-speed rotary tablet press, the procedure of the tablet press and the feeding cylinder are changed, single stamping is changed into 3-6 stamping, the feeding cylinder is fed by the original weight, the feeding cylinder is transversely pushed by a rotary rod to be matched with a screw rod to longitudinally convey and feed, a feeding host is started, the tablet press is started, the pressure parameter is 50KN, and the tablet with the diameter of 4mm and the thickness of 3mm is obtained.
Comparative example 5
The same formulation as in example 1 was used, except that the pressure parameter in comparative example 5 was 30KN.
Comparative example 6
The same formulation as in example 1 was used, except that the components of comparative example 6 were not uniformly stirred using a three-dimensional mixer.
Comparative example 7
The same formulation as in example 1 was used except that the components of comparative example 7 were not dried, and the moisture was found to be 7%.
Comparative example 8
The same formulation as in example 1, except that the tablet press (cold press process) of comparative example 8 was not fed screw-assisted and was only subjected to a single press.
Comparative example 9
The same formulation as comparative example 1, except that the tablet press (cold press process) of comparative example 9 was not subjected to screw-assisted feeding, and was subjected to only a single punching.
Test case
Taking the prepared polyhydroxyalkanoate tablet, and detecting conventional technical indexes: indentation hardness, crushing strength, friability and appearance, test method and performance requirements are as follows:
(1) Indentation hardness: according to Rockwell Hardness (HR), it is generally believed that an indentation hardness greater than 20N has no effect on shipping storage and subsequent use;
(2) Crushing strength: the method is carried out by using a single-grain compressive strength tester, the larger the numerical value is, the better the crushing strength of the tablet is, and the crushing strength is generally considered to be more than 30N and has no influence on transportation, storage and subsequent use;
(3) Friability: according to the friability checking method of the tablet according to the three general rules 0923 of Chinese pharmacopoeia, the particles are required to roll for 100 times in a friability checking instrument, the ratio of the loss weight to the original weight is friability, and the friability is more than 1%, namely unqualified;
(4) Appearance: the visual inspection method is carried out according to the part 1 of the SH/T1541.1-2019 plastic particle appearance test method, and the qualification standard is that the appearance of the particles is visually smooth, has no obvious holes, is rough and the like.
The test results of examples 1 to 5 and comparative examples 1 to 9 are shown in Table 2.
TABLE 2
As can be seen from the experimental results in Table 2, the polyhydroxyalkanoate tablets prepared in examples 1 to 5 have high indentation hardness, high crushing strength, low friability, and smooth appearance. The strength and hardness of the tablets can affect the application of subsequent tablet products, for example, when the resulting tablet product and other materials are subjected to further modified mixing, a high-speed mixer is required, if the strength and hardness are insufficient, the tablets can be stirred and broken into powder, the powder state is unfavorable for the next feeding into a processing machine, and a plurality of inconveniences can be caused in the transportation process.
In comparative example 1, the polyhydroxyalkanoate powder was used in a conventional tablet press (cold press process), and since the pure polyhydroxyalkanoate powder was extremely poor in flowability, even if the optimized processes such as three-time punching and auxiliary feeding were used, the form of the cold-pressed tablet was still incomplete, and the polyhydroxyalkanoate tablet was easily dispersed under force, and was also dispersed into powder when stored and transported.
Examples 1 and 4 compare the effect of calcium carbonate and magnesium stearate on the appearance of tablets, and experiments prove that the use of calcium carbonate and magnesium stearate can improve the appearance of tablets and make the appearance of tablets smoother while maintaining the tablets and hardness. And the demoulding is facilitated during processing, and the cold pressing processing is facilitated.
Comparative example 2 and comparative example 4 comparative octenyl succinic acid starch ester influence on tablet hardness, strength and friability, experiments prove that octenyl succinic acid starch ester helps to improve tablet strength and hardness, and does not have significant influence on tablet friability.
Comparative example 3 and comparative example 4 comparative carboxymethyl starch and maltodextrin affect tablet hardness, strength and friability, and experiments demonstrate that anionic carboxymethyl starch and maltodextrin help to increase tablet strength and hardness, but tablet friability increases slightly.
Comparative example 5, comparative example 6 and example 1 respectively compare the influence of the pressure parameters and the pre-mixing step on the tablets, and experiments prove that proper pressure and the use of a three-dimensional mixer to stir the components uniformly in advance are more conducive to improving the hardness, strength and smoothness of the appearance of the tablets, and meanwhile ensure that the friability of the tablets meets the requirements.
Comparison of comparative example 7 with example 1 shows that moisture has a great influence on the hardness of the tablet, and is embodied in that after a period of time, the moisture in the tablet is reduced, the viscosity of the material is not previously great, and the hardness is reduced or directly loosened.
Comparison of comparative example 8 with example 1, and comparison of comparative example 9 with comparative example 1, shows that the combination of multiple punches and screw assisted feeding by the tablet press is more conducive to improving tablet hardness, strength, reducing tablet friability, and ensuring satisfactory smoothness of appearance. The feeding cylinder uses the rotary rod to transversely push and match with the screw rod to carry out longitudinal conveying, so that the feeding continuity of the powder material can be better ensured, and the powder can be fully filled into the die.
The above-described embodiments of the present invention have been described in detail, but the present invention is not limited to the above-described embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (13)
1. The polyhydroxyalkanoate tablet is characterized by comprising the following components in parts by weight:
60-80 parts of polyhydroxyalkanoate;
1-10 parts of maltodextrin;
1-10 parts of carboxymethyl starch;
1-15 parts of octenyl succinic acid starch ester;
1-15 parts of a lubricant;
the lubricant includes magnesium stearate and calcium carbonate;
the preparation method of the polyhydroxyalkanoate tablet comprises the following steps:
pretreating each component, and putting the pretreated components into a vacuum microwave drying oven for drying so that the moisture of the powder material is not more than 0.5%; then the components are put into a three-dimensional mixer according to the proportion and are mixed uniformly; putting the uniformly mixed powder into a feeding cylinder of a high-speed rotary tablet press, changing the procedure of the tablet press and the feeding cylinder, changing single stamping into 3-6 times of stamping, discharging the feeding cylinder from the original weight, changing the feeding cylinder into a rotary rod for transverse pushing, matching with a screw rod for longitudinal conveying feeding, starting a feeding host, and starting the tablet press;
the pressure range adopted by the stamping is 40-60KN.
2. The polyhydroxyalkanoate tablet of claim 1, wherein the polyhydroxyalkanoate comprises 60-80% of the polyhydroxyalkanoate tablet by weight.
3. The polyhydroxyalkanoate tablet of claim 2, wherein the polyhydroxyalkanoate comprises 60-70% by weight of the polyhydroxyalkanoate tablet.
4. The polyhydroxyalkanoate tablet of claim 1, wherein the maltodextrin comprises 1-10% by weight of the polyhydroxyalkanoate tablet.
5. The polyhydroxyalkanoate tablet of claim 4, wherein the maltodextrin comprises 5-10% by weight of the polyhydroxyalkanoate tablet.
6. The polyhydroxyalkanoate tablet of claim 1, wherein the carboxymethyl starch comprises 1-10% by weight of the polyhydroxyalkanoate tablet.
7. The polyhydroxyalkanoate tablet of claim 6, wherein the carboxymethyl starch comprises 5-10% by weight of the polyhydroxyalkanoate tablet.
8. The polyhydroxyalkanoate tablet of claim 1, wherein the starch octenyl succinate comprises 1-15% by weight of the polyhydroxyalkanoate tablet.
9. The polyhydroxyalkanoate tablet of claim 8, wherein the starch octenyl succinate comprises 10-15% by weight of the polyhydroxyalkanoate tablet.
10. The polyhydroxyalkanoate tablet of claim 1, wherein the lubricant comprises 1-15% by weight of the polyhydroxyalkanoate tablet.
11. The polyhydroxyalkanoate tablet of claim 10, wherein the lubricant comprises 10-15% by weight of the polyhydroxyalkanoate tablet.
12. The polyhydroxyalkanoate tablet according to claim 1, wherein the tablet has a diameter in the range of 3-25mm and a thickness in the range of 3-8mm.
13. Use of the polyhydroxyalkanoate tablet of any one of claims 1-12 in the fields of food packaging, cosmetic packaging, and pharmaceutical packaging.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102186916A (en) * | 2008-10-13 | 2011-09-14 | 罗盖特公司 | Elastomeric compositions based on esters of a starchy material and method for preparing such compositions |
| KR20210111186A (en) * | 2021-07-30 | 2021-09-10 | 씨제이제일제당 (주) | Biodegradable resin composition, biodegradable film and biodegradable articles using same |
| CN113845714A (en) * | 2021-11-20 | 2021-12-28 | 郑州市彦峰塑料包装有限公司 | Green environment-friendly packaging bag and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102186916A (en) * | 2008-10-13 | 2011-09-14 | 罗盖特公司 | Elastomeric compositions based on esters of a starchy material and method for preparing such compositions |
| KR20210111186A (en) * | 2021-07-30 | 2021-09-10 | 씨제이제일제당 (주) | Biodegradable resin composition, biodegradable film and biodegradable articles using same |
| CN113845714A (en) * | 2021-11-20 | 2021-12-28 | 郑州市彦峰塑料包装有限公司 | Green environment-friendly packaging bag and production method thereof |
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