CN109738610A - A kind of method of Fast Evaluation lignocellulose castoff compost rotten degree - Google Patents
A kind of method of Fast Evaluation lignocellulose castoff compost rotten degree Download PDFInfo
- Publication number
- CN109738610A CN109738610A CN201811572020.0A CN201811572020A CN109738610A CN 109738610 A CN109738610 A CN 109738610A CN 201811572020 A CN201811572020 A CN 201811572020A CN 109738610 A CN109738610 A CN 109738610A
- Authority
- CN
- China
- Prior art keywords
- solution
- compost
- added
- acid
- content
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Fertilizers (AREA)
Abstract
The invention discloses a kind of methods of Fast Evaluation lignocellulose castoff compost rotten degree.This method calculates the ratio of cellulose and content of lignin by measuring cellulose and content of lignin in compost respectively, determines the rotten degree of compost.This method can rapidly and accurately monitor the rotten degree in composting process, be conducive to be monitored in time in compost maturity and arrive, reduce the unnecessary compost time.This method is easy to operate and fast and effective, can be obviously shortened detection cycle, while without using expensive instrument, low in cost, has more general applicability.
Description
Technical field
The present invention relates to organic fertilizer field more particularly to a kind of Fast Evaluation lignocellulose castoff compost rotten degrees
Method.
Background technique
Lignocellulosic waste has high organic, is not likely to produce smell, good physical property and low heavy metal etc.
Feature.It as soil conditioner is a wise selection using containing high lignocellulosic waste.However, directly application can be led
The generation for causing the noxious materials such as ethyl alcohol, organic acid and phenols, causes plant growth to be obstructed.Take the biodegradable side of aerobic fermentation
Formula stabilizes these substances, is one of elimination or the usual way for correcting its potential hazard, may advantageously facilitate ecology and follow
Ring.
Compost is a humification process, is the process for making unstable organic matter be transformed into stable organic matter, not at
Contain a large amount of noxious materials in ripe or fresh compost, environment can be endangered after application, compost maturity, which is that soil is practical, answers
With a key index of change.
Common compost maturity index such as carbon-nitrogen ratio (C/N), moisture content, organic matter, Water Soluble Organic Carbon (TOC) and kind
Sub- germination index (GI) etc..However, lignocellulose waste contains very high C/N, cellulose and lignin etc., it can not be quick
It is decomposed by the microorganisms, general maturity indexes such as C/N, organic matter etc. are unsuitable for evaluating its compost maturity.GI then used time ratio
It is longer to be unfavorable for quickly measuring, and lignocellulose substance toxicity is low, GI index is also less properly used as maturity indexes.This
Outside, TOC energy real-time monitoring rotten degree, but measurement needs to use expensive instrument, causes common laboratory that can not be measured.
Therefore, it is badly in need of the new maturity indexes of searching and is used as evaluation compost maturity, it is discarded for evaluation lignocellulose
Object compost has important practical significance.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of Fast Evaluation lignocellulose castoff compost rotten degree.
The technical solution used in the present invention is:
A kind of method of Fast Evaluation lignocellulose castoff compost rotten degree, includes the following steps:
1) content of cellulose in compost sample is measured, cellulose amount is obtained;
2) content of lignin in compost sample is measured, lignin amount is obtained;
3) ratio according to cellulose amount and lignin amount, determines the rotten degree of compost.
Preferably, the measurement of above-mentioned content of cellulose includes the following steps:
A) N g compost sample is added in nitration mixture, pickling removes precipitating, drying, obtains substance A;
B acid potassium bichromate solution) is added in substance A, liquor kalii iodide is added afterwards, adds the thio sulphur that concentration is K
Acid sodium solution has just shown blue to solution and half a minute is colour-fast, and the volume of record consumption hypo solution is b;
C step A) is repeated) and step B), but sample is not added, as blank control, record consumption hypo solution
Volume be a;
D the content of cellulose in sample) is calculated.
Preferably, the calculation formula of the content of above-mentioned cellulose is
Preferably, above-mentioned nitration mixture is acetic acid and nitric acid.
Preferably, the mass percent of above-mentioned acetic acid is 3~15%;It is highly preferred that the mass percent of acetic acid be 4~
6%.
Preferably, the mass percent of above-mentioned nitric acid is 1~10%;It is highly preferred that the mass percent of nitric acid be 3~
7%.
Preferably, the volume ratio of above-mentioned acetic acid and nitric acid is 1:(1~3).
It is highly preferred that the volume ratio of above-mentioned acetic acid and nitric acid is 1:1.
Preferably, step A) in pickling temperature be 80~100 DEG C, pickling time be 20~40min.
It is highly preferred that step A) in pickling temperature be 100 DEG C, pickling time be 25~35min.
Preferably, step B) in acid potassium bichromate solution be sulfuric acid that mass percent is 8~12% and concentration is
The mixed solution of the potassium bichromate of 0.05~0.2mol/L.
Preferably, the volume ratio of sulfuric acid and potassium bichromate is (1~2): (1~2);More preferably 1:1.
Preferably, step B) in the reaction time of substance A and acid potassium bichromate be 10~20min.
Preferably, the mass percent of above-mentioned liquor kalii iodide is 15~25%.
Preferably, the measurement of above-mentioned content of lignin includes the following steps:
I) M g sample is added in acid solution, obtains sediment;
II) acid solution is added in sediment to be cleared up, barium chloride solution, the rear acid potassium bichromate, again of being added is added
The sodium thiosulfate that addition liquor kalii iodide, rear addition concentration are F has just shown rufous and non-discolouring in half a minute, addition to solution
Starch solution is added the hypo solution that concentration is F and disappears to solution blue and show bright green, and record consumes thio sulphur
The volume of acid sodium solution is h;
III) step I is repeated) and step II), but sample is not added, as blank control, record consumption sodium thiosulfate is molten
The volume of liquid is s;
IV) content of lignin in sample is calculated.
Preferably, the calculation formula of the content of above-mentioned lignin are as follows:
Preferably, step II) digestion condition be room temperature, digestion time be 12~for 24 hours;It is highly preferred that digestion time is
15~18h.
The mass percent of acid solution is 0.5~5% in preferably: step I);Step II) in acid solution quality percentage
Number is 60~80%.
It is highly preferred that step I) in acid solution mass percent be 0.5~2%;Step II) in acid solution quality hundred
Score is 70~75%.
Preferably, step I) in acid solution be selected from acetic acid.
Preferably, step II) in acid solution be selected from sulfuric acid.
Preferably, step I) in precipitating further include the steps that being washed, dry;Preferably, ethyl alcohol and ether are utilized
Mixed liquor washed.
Preferably, the mass percent of above-mentioned barium chloride solution is 5~15%.
Preferably, step II) in acid potassium bichromate solution be sulfuric acid that mass percent is 8~12% and concentration is
The mixed solution of the potassium bichromate of 0.01~0.2mol/L.
Preferably, the volume ratio of sulfuric acid and potassium bichromate is (1~2): (1~2);More preferably 1:1.
Preferably, step II) in potassium iodide mass percent be 15~25%.
Preferably, step II) in starch solution mass percent be 0.5~2%.
Preferably, step II) in sodium thiosulfate concentration be 0.1~0.5mol/L;It is highly preferred that sodium thiosulfate
Concentration is 0.2mol/L.
Preferably, when the ratio of cellulose amount and lignin amount no longer changes, compost is decomposed.
The beneficial effects of the present invention are:
1, the present invention provides a kind of method for evaluating lignocellulose castoff compost rotten degree, this method can be fast
Rotten degree in fast monitor composting process is conducive to be monitored in time in compost maturity and arrive, reduces unnecessary heap
The fertile time.
2, method of the invention is easy to operate and fast and effective, can be obviously shortened detection cycle, while high without using
Expensive instrument, it is low in cost, have more general applicability.
Detailed description of the invention
Fig. 1 is the ratio of cellulose amount and lignin amount with the change curve of compost time;
Fig. 2 is change curve of the Water Soluble Organic Carbon content in lignocellulose castoff compost with the compost time
Figure;
Fig. 3 is trend chart of the seed germination index with the compost time;
Fig. 4 is the ratio of cellulose amount and lignin amount and the correlation curve of Water Soluble Organic Carbon content;
Fig. 5 is the ratio of cellulose amount and lignin amount and the correlation curve of seed germination index.
Specific embodiment
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art are according to the present invention
Some nonessential modifications and adaptations that the principle of elaboration is made all belong to the scope of protection of the present invention.Following specific works of example
Skill parameter etc. is also only an example in OK range, i.e. those skilled in the art can do suitable model by the explanation of this paper
Interior selection is enclosed, and does not really want to be defined in hereafter exemplary specific data.
Compost model:
Composting material is the vinifera waste residue (200Kg) of grape wine brewery, and moisture content is adjusted to about 60%, at PVC barrels
Composting 180 days in type compost reactor;
Primary every turning in three days, after 60 days, each week turning is once to keep oxygen content in fertile heap to reach Institute of Micro-biology
Aerobic gas;
Acquisition sample is primary within every 20 days, to obtain objectively analysis as a result, taking the sample of 3 differences of compost respectively
It is tested and analyzed, every part of sample 200g.
Embodiment
A kind of method of Fast Evaluation lignocellulose castoff compost rotten degree, includes the following steps:
1) content of cellulose in compost sample is measured:
A the compost sample after) air-drying 1g is slowly put into the mixed solution of acetic acid and nitric acid the (volume of acetic acid and nitric acid
The ratio between be 1:1, the mass percent of acetic acid is 5%, and the mass percent of nitric acid is the 5%) pickling in 100 DEG C of boiling water bath
Solution addition water after pickling is diluted and is centrifuged 2~3 times, taken precipitating to dry, obtain substance A by 30min;
B the acid potassium bichromate (weight that the sulfuric acid and concentration that mass fraction is 10% are 0.1mol/L) is added in substance A
The volume ratio of the mixed liquor of potassium chromate, sulfuric acid and potassium bichromate: 1:1), 15min is aoxidized, the KI that mass percent is 20% is added
Solution, after with the sodium thiosulfate that concentration is 0.2mol/L be titrated to solution just show blue and half a minute in it is non-discolouring, record sulphur
The consumption volume of sodium thiosulfate solution is b;
C step A) is repeated) and step B), but sample is not added, as blank control, record disappearing for hypo solution
Consumption volume is a;
D the content of cellulose in sample) is calculated, calculation formula is as follows:
Wherein, K is the concentration of hypo solution, mol/L;
A is step C), it may be assumed that the volume of sodium thiosulfate consumed by blank titration, mL;
B is step B), it may be assumed that solution titrates the volume of consumed sodium thiosulfate, mL;
N is the quality of compost sample, g;
24 be 1mol C6H10O5It is equivalent to the molal quantity of sodium thiosulfate;
2) content of lignin in compost sample is measured:
I) compost sample after air-drying 1g is added in the acetum that mass percent is 1%, and centrifugation removes supernatant
Liquid obtains sediment;
II) it is washed repeatedly sediment 3-4 times using the mixed liquor of ethyl alcohol and ether, rear drying is added mass percent and is
72% sulfuric acid clears up 16h in room temperature, and distilled water water-bath 3min in digestion solution is added, and it is 10% that mass percent, which is added,
Barium chloride solution is centrifuged and retains sediment, rear that the sulfuric acid that mass percent is 10% and the weight that concentration is 0.025mol/L is added
All substances are simultaneously transferred in conical flask by potassium chromate mixed liquor water-bath 15min in sediment, cooling, and mass percent is added
For 20% liquor kalii iodide, sodium thiosulfate to the solution that concentration is 0.2mol/L is added is just aobvious brownish red and in half a minute
It is non-discolouring, starch solution is added, the hypo solution that concentration is 0.2mol/L is added and disappears and shows bright to solution blue
Green, the consumption volume for recording hypo solution is h;
III) step I is repeated) and step II), but sample is not added, as blank control, record hypo solution
Disappear
Consumption volume is s;
IV) content of lignin in sample is calculated, calculation formula is as follows:
Wherein, F is the concentration of sodium thiosulfate, mol/L;
S is step III), it may be assumed that the volume of sodium thiosulfate consumed by blank titration, mL
H is step II), it may be assumed that solution titrates the volume of consumed sodium thiosulfate, mL;
M is the quality of compost sample, g;
48 be 1mol C11H12O4It is equivalent to the titer of sodium thiosulfate (concentration 0.2mol/L);
3) ratio (CH) for calculating cellulose and lignin, determines the rotten degree of compost.
The CH value of different composting periods is measured using the above method, rear CH value of drawing is with the curve of compost time change, knot
Fruit such as Fig. 1:
As shown in Figure 1: the CH value of compost constantly declines with the extension of compost time, and to after 160 days, CH value becomes compost
In gentle, after no longer change substantially.
Comparative example 1
The method for determining wood fibre compost maturity by the content of Water Soluble Organic Carbon (TOC) in measurement compost:
It is in mass ratio to be vibrated for 24 hours in the case where revolving speed is 150~200r/min after 1:10 is mixed with ultrapure water by compost sample,
8000~13000r/m is centrifuged 15min at 4 DEG C afterwards, and supernatant is crossed 0.45 μm of filter membrane, DOM solution is obtained, by TOC instrument
(TOC2V CPH, Shimadzu) measures total organic carbon amount.
The TOC value of different composting periods is measured by the above method, rear TOC value of drawing with the curve of compost time change,
As a result such as Fig. 2:
As shown in Figure 2: with the extension of compost time, the TOC value in compost also constantly declines, compost to after 160 days,
TOC value tends towards stability, after no longer change substantially, this is very close with the variation tendency of the CH value of embodiment 1.
Comparative example 2
The method for determining wood fibre compost maturity by seed germination index (GI):
It takes 5mL compost extracting solution to be added in the culture dish equipped with filter paper, selects 20 oenanthe stolonifera seeds and be put into culture dish
And evenly spread out, in 25 ± 1 DEG C constant incubator culture 3 days, in the seed of germination seed root long lower than 2mm not counting germinate,
The calculation formula of seed germination index (GI) are as follows:Ultrapure water replaces compost extracting solution as control
Group;
Wherein, G is experimental group germination percentage;L is experimental group seed root long;G0 is control group germination percentage;L0 is control group kind
Sub- root long.
The GI value of different composting periods is measured by the above method, the rear GI that draws is with the curve graph of compost time change, knot
Fruit sees Fig. 3:
As shown in Figure 3: in the initial phase of lignocellulose compost, GI index has reached 84.6%, if according to GI
Value shows that compost has reached decomposed judgment criteria for 80%, then lignocellulosic compost is decomposed at this time, also
It is to say, it is just decomposed by compost treatment to determine that lignocellulosic compost is not necessarily to by GI, this does not obviously meet convention, this
Also illustrate that seed germination index is unsuitable for judging the rotten degree of wood fibre compost.
The correlation of CH, TOC and GI:
As shown in Figure 4: the CH value and Water Soluble Organic Carbon method (TOC) of the different composting periods of the method for the present invention measurement measure
Result height it is consistent, the degree of correlation of the two reaches 0.998, this illustrate CH of the invention can effectively replace TOC method as wood
The evaluation index of matter cellulose compost maturity, and method of the invention is not necessarily to use expensive instrument;
As shown in Figure 5: the CH value of the compost of the different phase of the method for the present invention measurement is related to the result that GI method measures
Coefficient is very low, and only 0.197, and the obvious counterintuitive of result of GI method, this illustrates that GI method is not suitable as wood fibre
The judgement of compost maturity.
Claims (10)
1. a kind of method of Fast Evaluation lignocellulose castoff compost rotten degree, characterized by the following steps:
1) content of cellulose in compost sample is measured, cellulose amount is obtained;
2) content of lignin in compost sample is measured, lignin amount is obtained;
3) ratio according to cellulose amount and lignin amount, determines the rotten degree of compost.
2. according to the method described in claim 1, it is characterized by: the measurement of the content of cellulose includes the following steps:
A) N g compost sample is added in nitration mixture, pickling removes precipitating, drying, obtains substance A;
B acid potassium bichromate solution) is added in substance A, liquor kalii iodide is added afterwards, adds the sodium thiosulfate that concentration is K
Solution has just shown blue to solution and half a minute is colour-fast, and the volume of record consumption hypo solution is b;
C step A) is repeated) and step B), but sample is not added, as blank control, the body of record consumption hypo solution
Product is a;
D the content of cellulose in sample) is calculated.
3. according to the method described in claim 2, it is characterized by: the calculation formula of the content of the cellulose is
4. according to the method in claim 2 or 3, it is characterised in that: step A) in nitration mixture be acetic acid and nitric acid;It is preferred that
, the mass percent of the acetic acid is 3~15%, and the mass percent of the nitric acid is 1~10%;Preferably, the vinegar
The volume ratio of acid and nitric acid is 1:1~3.
5. according to the method in claim 2 or 3, it is characterised in that: step A) in pickling temperature be 80~100 DEG C, acid
Washing the time is 20~40min.
6. according to the method described in claim 1, it is characterized by: the measurement of the content of lignin includes the following steps:
I) M g sample is added in acid solution, obtains sediment;
II) acid solution is added in sediment to be cleared up, barium chloride solution, the rear acid potassium bichromate solution, again of being added is added
Liquor kalii iodide, rear addition concentration is added and has just shown non-discolouring in blue and half a minute to solution for the sodium thiosulfate of F, shallow lake is added
Powder solution is added the hypo solution that concentration is F and disappears to solution blue and show bright green, record consumption thiosulfuric acid
The volume of sodium solution is h;
III) step I is repeated) and step II), but sample is not added, as blank control, record consumes hypo solution
Volume is s;
IV) content of lignin in sample is calculated.
7. according to the method described in claim 6, it is characterized by: the calculation formula of the content of the lignin are as follows:
8. method according to claim 6 or 7, it is characterised in that: step II) digestion condition be room temperature, digestion time
For 12~for 24 hours.
9. method according to claim 6 or 7, it is characterised in that: step I) in acid solution mass percent be 0.5~
5%;Step II) in acid solution mass percent be 60~80%.
10. according to the method described in claim 1, it is characterized by: when the ratio of cellulose amount and lignin amount no longer changes
When, compost is decomposed.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811572020.0A CN109738610A (en) | 2018-12-21 | 2018-12-21 | A kind of method of Fast Evaluation lignocellulose castoff compost rotten degree |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811572020.0A CN109738610A (en) | 2018-12-21 | 2018-12-21 | A kind of method of Fast Evaluation lignocellulose castoff compost rotten degree |
Publications (1)
Publication Number | Publication Date |
---|---|
CN109738610A true CN109738610A (en) | 2019-05-10 |
Family
ID=66359494
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201811572020.0A Pending CN109738610A (en) | 2018-12-21 | 2018-12-21 | A kind of method of Fast Evaluation lignocellulose castoff compost rotten degree |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109738610A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111157677A (en) * | 2019-12-19 | 2020-05-15 | 江苏大学 | Organic waste stacking fermentation decomposition degree evaluation method |
CN111175291A (en) * | 2020-01-15 | 2020-05-19 | 重庆工商大学 | Method for rapidly detecting compost maturity |
CN112033850A (en) * | 2020-09-17 | 2020-12-04 | 青岛兴开环境科技有限公司 | Method for evaluating degree of decomposition of materials in fermentation tank in production process |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101806738A (en) * | 2010-04-27 | 2010-08-18 | 南京农业大学 | Method for fast characterizing compost maturity |
CN103868778A (en) * | 2014-04-02 | 2014-06-18 | 兰州大学 | Method for measuring lignin content of herbaceous plants |
CN104237453A (en) * | 2014-09-30 | 2014-12-24 | 云南瑞升烟草技术(集团)有限公司 | Method for measuring content of cellulose in tobacco |
CN108254327A (en) * | 2018-01-24 | 2018-07-06 | 上海理工大学 | The improved method of lignocellulose biomass component analysis |
-
2018
- 2018-12-21 CN CN201811572020.0A patent/CN109738610A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101806738A (en) * | 2010-04-27 | 2010-08-18 | 南京农业大学 | Method for fast characterizing compost maturity |
CN103868778A (en) * | 2014-04-02 | 2014-06-18 | 兰州大学 | Method for measuring lignin content of herbaceous plants |
CN104237453A (en) * | 2014-09-30 | 2014-12-24 | 云南瑞升烟草技术(集团)有限公司 | Method for measuring content of cellulose in tobacco |
CN108254327A (en) * | 2018-01-24 | 2018-07-06 | 上海理工大学 | The improved method of lignocellulose biomass component analysis |
Non-Patent Citations (1)
Title |
---|
瞿贤等: "生物反应器填埋条件下垃圾生物质组分的初期降解", 《环境科学学报》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111157677A (en) * | 2019-12-19 | 2020-05-15 | 江苏大学 | Organic waste stacking fermentation decomposition degree evaluation method |
CN111175291A (en) * | 2020-01-15 | 2020-05-19 | 重庆工商大学 | Method for rapidly detecting compost maturity |
CN112033850A (en) * | 2020-09-17 | 2020-12-04 | 青岛兴开环境科技有限公司 | Method for evaluating degree of decomposition of materials in fermentation tank in production process |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Gao et al. | Effects of long-term green manure application on the content and structure of dissolved organic matter in red paddy soil | |
Olk et al. | Changes in chemical properties of organic matter with intensified rice cropping in tropical lowland soil | |
CN109738610A (en) | A kind of method of Fast Evaluation lignocellulose castoff compost rotten degree | |
CN106495770A (en) | A kind of efficient high-rate composting fermentation process of utilization agriculture and forestry organic waste material | |
JP4650374B2 (en) | Method for judging compost maturity and solution for judgment | |
CN103725669A (en) | High-throughput screening method for high-yield monascus pigment strain | |
CN110967305A (en) | Test paper box for rapidly detecting compost maturity and using method thereof | |
Ma et al. | Interactive effects of crop residue quality and nitrogen fertilization on soil organic carbon priming in agricultural soils | |
JP2008051618A5 (en) | ||
Li et al. | Evaluation of no-tillage impacts on soil respiration by 13C-isotopic signature in North China Plain | |
Paradelo et al. | Can stability and maturity be evaluated in finished composts from different sources? | |
CN112299924A (en) | Novel efficient biochemical potassium fulvate and preparation method thereof | |
Aslam et al. | Predicting phytotoxicity of compost-amended soil from compost stability measurements | |
CN112110762A (en) | Water-soluble fertilizer and production process thereof | |
CN108490122B (en) | Pit quality assessment method | |
CN108562471B (en) | Method for rapidly detecting activity of plant root system | |
CN114375637A (en) | Wheat seed germination and seedling stage regulation and control method based on fulvic acid spectroscopy characteristics | |
CN111766335B (en) | Method for judging compost maturity | |
Brinton et al. | Plant performance in relation to oxygen depletion, CO2-rate and volatile fatty acids in container media composts of varying maturity | |
CN112540166A (en) | Method for rapidly determining microbial biomass nitrogen in forest soil by using carbon nitrogen analyzer | |
CN110669606A (en) | Organic pit mud for brewing wine and preparation process thereof | |
CN105248452B (en) | Alfalfa is kept a full stand of seedings type seed coat agent and preparation method and application | |
Kumari et al. | Effect of different soil conservation practices on soil microbial biomass carbon, nitrogen and phosphorus under rice based cropping system in Bihar | |
Kong et al. | Applicability and limitation of compost maturity evaluation indicators: A review | |
CN103125280A (en) | Safety monitoring alarm method of cadmium (Cd) in rice |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190510 |
|
RJ01 | Rejection of invention patent application after publication |